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Technical Guide

Operating Hints for


Using Split/Splitless
Injectors
Inside:
Overviews of split and splitless
injection techniques

Backpressure-regulated injection
systems

Headpressure-regulated injection
systems

Operating in the split injection mode

Inlet liners for split injections

Operating in the splitless injection


Mode

Inlet liners for splitless injections

Septum purge optimization

Problems associated with split and


splitless injections

Direct injection as an alternative to


splitless injection

Hints for analyzing dirty samples

Hints for performing routine injection


port maintenance

Product listing

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Table of Contents Overview of Split/Splitless Injection Techniques


Overview of Split/Splitless Injection In capillary and micropacked gas chromatography (GC) there are four primary techniques
Techniques ......................................2 for vaporizing a sample and transferring it onto the inlet of the analytical column: split, split-
Backpressure-Regulated Injection Systems ..2 less, direct, and on-column injections. Of these, split and splitless injections are the most
Headpressure-Regulated Injection
Systems..........................................3
commonly used techniques. This technical guide focuses on split and splitless injections—
Operating in the Split Injection Mode ......4 their optimization, troubleshooting, and system maintenance.
Inlet Liners for Split Injectors ................6
Operating in the Splitless Injection Mode ..7 Split and splitless injections are techniques that introduce the sample into a heated injection
Solvent Focusing and Analyte Focusing ......9 port as a liquid, and then rapidly and completely vaporize the sample solvent as well as all of
Inlet Liners for Splitless Injections ........11 the analytes in the sample. The vaporized sample is transferred to the head of the column.
Septum Purge Optimization ..................12
Problems Associated with Split and Splitless In the split injection mode, only a fraction of the vaporized sample is transferred onto the head
Injections ......................................13 of the column. The remainder of the vaporized sample is removed from the injection port via
Thermal Decomposition . . . . . . . . . . . . . .13
Active Compounds . . . . . . . . . . . . . . . . . .13 the split vent line. Split injections should be used only when sample concentrations are high
Molecular Weight Discrimination . . . . . . .13 enough to allow a portion of the sample to be discarded during the injection process, while still
Needle Discrimination . . . . . . . . . . . . . . .14 maintaining a sufficient concentration of analytes at the detector to produce a signal.
Backflash . . . . . . . . . . . . . . . . . . . . . . . . .15
Sample Size and Injection Port When target analyte concentrations are so low that splitting the sample in the injection port
Temperature . . . . . . . . . . . . . . . . . . . . .15 will not allow an adequate signal from the detector, the injector should be operated in the
Optimizing the Rate of Injection . . . . . . . .16
Pressure Programming . . . . . . . . . . . . . .16 splitless injection mode. In the splitless injection mode, most of the vaporized sample is
Direct Injection as an Alternative to Splitless transferred to the head of the column.
Injection ........................................16
Hints for Analyzing Dirty Samples ..........18 The process of performing either a split or splitless injection is controlled by changing the
Hints for Performing Routing Injection Port flow path and flow rate of carrier gas through the injection port. The position of a switching
Maintenance ..................................19 valve in the injection port determines the flow path. In split injections, a high carrier gas
Cleaning and Deactivating Injector Liners . .19
flow rate rapidly moves the vaporized sample through the injection port liner, past the col-
Replacing Critical Seals . . . . . . . . . . . . . .19
Changing Septa . . . . . . . . . . . . . . . . . . . .19 umn (with only a minimal amount directed to the head of the column), and out the split vent.
Product Listing ........4, 5, 9, 18, 19, 20–35 In splitless injections, a relatively slow carrier gas flow rate directs most of the vaporized
Restek Flowmeter 6000 . . . . . . . . . . . . . . .4 sample into the head of the column.
Soap Film Bubble Flowmeters . . . . . . . . . . .4
Split Vent Trap . . . . . . . . . . . . . . . . . . . . . .5 Split/splitless injection ports can be either backpressure-regulated or headpressure-regulated
Methane Cylinder . . . . . . . . . . . . . . . . . . . .5 systems. Most modern GCs are backpressure regulated. However, some GC manufacturers
Split and Splitless Injection in Capillary
GC, 4th Ed. book . . . . . . . . . . . . . . . . . . .9 still find headpressure regulation advantageous and use this design in their split/splitless
Mini Wool Puller/Inserter . . . . . . . . . . . . .18 injectors. It is important for analysts to be familiar with their injection port hardware and the
Nylon Tube Brushes and Pipe Cleaner . . . .19 operating principles of their instruments, so that they factor in the variables affecting the
Leak Detective II Leak Detector . . . . . . . . .19 accuracy and reproducibility of their results.
Siltek™ Inlet Liners . . . . . . . . . . . . . . . . . .20
Base-Deactivated Inlet Liners . . . . . . . . . .20
Prepacked Liners . . . . . . . . . . . . . . . . . . .20
Liners for Agilent/Finnigan GCs . . . . . .21–22 Backpressure-Regulated Injection Systems
O-rings . . . . . . . . . . . . . . . . . . . . . . . . . .23 Figure 1 illustrates the components of a typical backpressure-regulated split/splitless injection
Inlet & FID Maintenance Kits . . . . . . . . . .23 system (e.g., Agilent 5890, 6850, 6890 GCs; Varian 3300, 3400, 3500, 3600, 3800 GCs;
Vespel® Ring Inlet Seals for Agilent Shimadzu 17A GCs). A flow controller, positioned upstream from the injection port, controls the
5890/6890 and 6850 GCs . . . . . . . . . . .24
Rethreading Tool . . . . . . . . . . . . . . . . . . .24 total amount of carrier gas that enters the injection port. A backpressure regulator, located down-
Replacement Inlet Seals . . . . . . . . . . . . . .25 stream from the injection port body, regulates the pressure inside the injection port. Carrier gas
Replacement Inlet Cross-Disk Seal flow rate in the column is determined by the pressure that is maintained in the injection port. The
for Agilent GCs . . . . . . . . . . . . . . . . . . .25 outlet of the backpressure regulator is the outlet of the split vent line. The split vent line outlet is
Liners for Varian GCs . . . . . . . . . . . . .26–27
at the ambient pressure of the laboratory. The flow controller and the backpressure regulator work
Varian Inlet Liner Seals . . . . . . . . . . . . . .27
Inlet Liner Removal Tool . . . . . . . . . . . . .27 together to determine the column flow rate, septum purge flow rate, and split vent flow rate.
Liners for PerkinElmer GCs . . . . . . . . . . .28
Liners for Shimadzu GCs . . . . . . . . . . . . .29 Split and splitless injections in backpressure-regulated systems are controlled by the position
Liners for Thermo Finnigan GCs . . . . .30–31 of the 3-way solenoid valve. In the split injection mode, the flow path is always open from
Inlet Liner Seal for TRACE™ 2000 GCs . . . .31 the injection port body through the 3-way solenoid valve to the split vent line. In the splitless
Graphite Sealing Ring and Washer for 8000 injection mode, the flow path is temporarily closed from the injection port body to the split
Series and TRACE™ GC Inlet Liners . . . . .31
Septa . . . . . . . . . . . . . . . . . . . . . . . . . . . .32 vent line. The carrier gas flow rate through the injection port liner is simply the column flow
Press-Tight® Connectors . . . . . . . . . . . . .33 rate. Any excess flow is directed through the septum purge line, into the 3-way solenoid
Polyimide Resin . . . . . . . . . . . . . . . . . . . .33 valve, and out the split vent line.
MXT®-Union Connector Kits . . . . . . . . . . .34
Valco® Connectors . . . . . . . . . . . . . . . . . .34 In backpressure-regulated systems, the split vent flow rate is changed by adjusting the flow
Gerstel GRAPHPACK® 3D/2 Connectors . .34 controller. An increase in the total flow being delivered to the injection port will result in a
Guard Columns and Transfer Lines . . . . . .35
higher split vent flow rate and a higher split ratio. Column flow rate is not affected by
changes in the total flow being delivered to the injection port, but by the backpressure regu-
www.restekcorp.com lator. To maintain the same pressure at all times, use the backpressure regulator to compen-
sate for a change in the total flow delivered to the injection port.
3

A flow-controlled, backpressure-regulated system is beneficial as it gives some measure of


protection against a catastrophic loss of carrier gas. If there is a leak at an injection port fit-
ting or a column fitting, the maximum rate of carrier gas loss would be the total flow rate
into the injection port as determined by the flow controller. Unlimited flow of carrier gas
into the injection port is prevented by having the flow controller at the inlet of the injection
port. Leaks are indicated by a failure to maintain split vent flow rate. A common mistake
analysts make when they observe a reduced split vent flow is to increase the total system
flow, rather than check for leaks at the injector and column fittings. By understanding the
characteristics of backpressure regulated pneumatics, analysts can detect and correct a leak,
to avoid poor chromatography.

Figure 1. Figure 1.
Split injection flowpaths in a typical flow-controlled/backpressure-regulated system. • All carrier gas except septum purge
injection needle flow directed through injector.
flow controller valve
port
• Column flow (established by backpres-
carrier gas septum sure regulator) enters column.
inlet purge vent
closed • Solenoid valve open from injector to split
vent. Bulk of gas flows out of injector
o-ring or
split vent liner, through solenoid valve, out split
ferrule
vent.
3-way solenoid
injector valve • Sample vapor is directed onto column or
liner
backpressure
vented through split vent and is split in
regulator the same proportions as for carrier gas.
• Split ratio = portion of sample vented
analytical
column from split vent/portion of sample that
to detector enters column.

Headpressure-Regulated Injection Systems


Figure 2 illustrates the components of a typical headpressure-regulated split/splitless injec-
tion system (e.g., PE Autosystem; Shimadzu 9A & 14A; Thermo Finnigan Trace 2000
GCs). A pressure regulator upstream from the injection port regulates or maintains the pres-
sure inside the injection port. The pressure regulator supplies an unlimited flow of carrier
gas until the desired pressure is reached. The pressure inside the injection port establishes
the carrier gas flow in the column and determines the column flow rate. Flows through the
split vent line and the septum purge line are controlled by needle valves or restrictors down-
stream from the injection port. The outlet pressure of the septum purge and split vent lines
is ambient pressure. As long as constant pressure is maintained in the injection port, needle
valves and restrictors will give constant flows.

Figure 2. Figure 2.
Split injection flowpaths in a typical headpressure-regulated system. • Solenoid valve open: column flow passes
throttling valve pressure into column, split flow exits through split
needle
(optional safety regulator vent.
injection port valve
device)
septum • Throttling valve guards against loss of
carrier inlet purge vent carrier gas caused by leaks in injection
open system.
split vent

o-ring or solenoid needle


ferrule valve valve
injector
liner
column

to detector www.restekcorp.com
4

An on/off solenoid valve is used in headpressure-regulated systems instead of the 3-way


Restek Flowmeter 6000 solenoid valve used in backpressure-regulated systems. The position of the solenoid valve
determines whether the injection port is operated in the split or splitless injection mode. In
the split injection mode, the solenoid valve is always in the open position and the carrier gas
is allowed to flow through the injection port liner and out the split vent line. In the splitless
injection mode, the solenoid valve is closed and the only flow through the injection port
liner is the column flow. The pressure regulator compensates for excess carrier gas flow
available when the solenoid valve closes.

The throttling valve upstream from the pressure regulator (Figure 2) is an optional compo-
nent not typically included by the chromatograph manufacturer. We recommend installing a
throttling valve (flow controller or needle valve) to guard against catastrophic loss of carrier
gas if a leak occurs at an injection port fitting or a column fitting. To adjust the throttling
valve, gradually close the valve, reducing the gas flow until it matches the requirements of
the injection system. When the column headpressure begins to decrease, the throttling valve
is closed too far.

Operating in the Split Injection Mode


• Calculates linear velocity based on col- When operating in the split injection mode (Figures 1 and 2), the solenoid valve is always
umn ID. open along the flowpath from the injection port body to the split vent. With the exception of
• Useful for measuring flows for N2, air, the septum purge flow, all of the carrier gas entering the injection port flows through the
He, H2, CO2, O2, Ar, 7.5% CH4/Ar. injection port liner and toward the head of the column. At the head of the column, the carrier
• Reads flow accurately from 0 to gas flow is split between two flow paths: a portion of the flow enters the column as the col-
500mL/min. (0–300mL/min. for CO ).2 umn flow rate, and the remaining carrier gas flow is allowed to escape from the injection
• Accuracy is 0.2mL/min. or +/- 2.5%. port, out the split vent line via the solenoid valve. The amount of flow entering the column
• Usable with inlet pressures up to 25psi. is determined by the pressure of the carrier gas inside the injection port and the dimensions
• Measures split flow and calculates split of the analytical column. The relative proportions of the split vent flow and the column flow
ratio. determine the split vent ratio.
• Automatic shut-off.
Samples completely vaporized in the injection port liner behave in the same fashion as the
Description qty. cat.# carrier gas; sample vapors are split in the same proportions as the carrier gas, thereby allow-
Restek Flowmeter 6000 ing only a fraction of the sample to be introduced into the head of the column. A 50-to-1
(9-volt battery-operated) ea. 21622 split ratio can be used as a starting point when developing split injection methods. Table I
Recalibration Service for shows the appropriate split vent flow rates for helium and hydrogen carrier gases when
Restek Flowmeter 6000 ea. 24618 using common capillary column IDs.

Table I.
Soap Film Bubble Flowmeters Typical split vent flow rates for 50-to-1 split ratio at optimum linear velocity when using
• 1mL flowmeter measures flows a 30-meter column at 40°C.
between 0.1 and 10cc/min. Column ID (mm)/Split Vent Flow Rate
• 50mL flowmeter designed for flows Carrier Gas 0.18 0.25 0.32 0.53
between 10 and 300cc/min.
helium* 25cc/min. 37.5cc/min. 55cc/min. 135cc/min.
• Both flowmeters come with a reser-
voir bulb, twenty-four inches of hydrogen** 50cc/min. 75cc/min. 110cc/min. 270cc/min.
1
/4-inch ID tubing, adaptor tubes for *optimum carrier gas linear velocity=20cm/sec.
1
/8-inch tubing and 0.53mm ID capil- **optimum carrier gas linear velocity=40cm/sec.
lary columns, and Velcro® fasteners.
Equation 1 shows how the split ratio is calculated. Split vent flow rates easily can be measured
using a standard electronic flowmeter (cat.# 21622). However, measuring low flow rates (from
0.3 to 5cc/min.) exiting a capillary column can be difficult unless a special low-volume bub-
blemeter (cat.# 20135) or a sensitive electronic flowmeter is used. If a low flow-measuring
device is not available, Equation 2 can be used to determine the approximate column flow.

Calculating the on-column concentration of analytes is necessary to ensure that the column
is not overloaded and is operating within its capacity limits. Although quantitative analysis
Description qty. cat.# does not require that the on-column concentration be known, exceeding column capacity
1mL Bubble Flowmeter ea. 20135 decreases resolution and reduces quantitative accuracy. Equation 3 illustrates how to calcu-
50mL Bubble Flowmeter ea. 20136 late the approximate on-column concentration in the split mode.

Setting the injection port temperature properly is critical for obtaining good peak shape and
www.restekcorp.com response. Injection port temperature must be hot enough to provide rapid vaporization of all
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Equation 1. High-Capacity Split


Calculating the split ratio.
Vent Trap
column flow + split vent flow • Reduces the release of hazardous
Split ratio = materials from the capillary split vent
column flow
into the lab.
Equation 2. • Lasts one month or 1,500 injections.
Calculating the approximate column flow rate. • Includes connecting lines and mount-
(π) (column radius in cm)2 (column length in cm) ing kit.
Flow =
dead volume time (min.)
where π = 3.14159
For example, a 30m x 0.53mm ID column operated at 20cm/sec. linear velocity (helium)
retains methane for 2.50 min., and therefore has a flow rate of 2.65cm3/min.: Description qty. cat.#
High-Capacity Split Vent
(3.14159) (0.0265cm) (3000cm)
2
Trap ea. 20698
Flow = = 2.65cm3/min.
2.50 min.
High-Capacity Split Vent
Trap 5-pk. 20699
Equation 3.
Calculating the approximate on-column concentration for split injections.
Concentration = concentration in sample (µg/µL) × sample vol. injected (µL)
split ratio

sample components. In the split injection mode, the residence time of the sample in the
injection port is very short because of the high carrier gas flow rate through the injection
port liner and out the split vent. As a result, vaporization must be completed as rapidly as
possible. However, injection port temperatures must not be so high that they cause sample
degradation.
For customer service, call
800-356-1688, ext. 3
(814-353-1300, ext. 3)
or call your local

Restek representative.
When set up properly, split injections are very reproducible. Samples introduced under con-
stant temperature, pressure, and flow conditions will vaporize and split consistently.

Split injections can be used for both qualitative and quantitative work. Internal or external
reference compounds are split under identical conditions compared to analytes in samples.
Any variations experienced by the sample also are experienced by the reference compounds
when the sample matrix and standard matrix match exactly. In general, split inlet liners are
designed to have added surface area to help with sample vaporization. Improved vaporiza- Methane Cylinder
tion can be acheived with changes in liner geometry that increase the surface area. Setting the column flow rate by injecting
Examples include incorporating fused silica or glass wool, CarboFrit™ packing, or using a methane and optimizing linear velocity
laminar cup. is a preferred method for establishing
reproducible retention times (ASTM
Method E1510-93). Measuring the lin-
ear velocity of your carrier gas is made
easy by using the Scotty® 14 cylinder
containing 1% methane in helium. The
Caution! complete kit includes the Scotty® 14
When analyzing hazardous compounds in the split mode, make sure they do not enter cylinder, a MINICYL regulator, a
the lab atmosphere through the split vent. A small, charcoal-filled split vent trap con- syringe adaptor, and a package of twenty
nected to the split vent protects you from breathing contaminated air (cat. # 20698). septa for the adaptor.

Description qty. cat.#


Complete Kit kit 20197
Replacement Septa 20-pk. 20198
Replacement Cylinder ea. 20199

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Inlet Liners for Split Injections


Split liners are designed with mixing chambers and tortuous flow paths, to fully vaporize the
sample into a homogeneous vapor cloud before it reaches the split point. All Restek split lin-
ers are fully deactivated using a high-temperature silanizing reagent. This caps surface
silanol groups so active compounds in the sample do not degrade or adsorb onto the hot
glass surface.
A
To trap non-volatile residue and prevent column contamination when analyzing dirty sam-
ples, pack split liners with wool, CarboFrit™ packing, or fused silica beads. Some of the
more commonly used inlet liners are described below.

B A) Split Liner with Wool D) Cup Splitter


The wool provides a large surface area to allow The sample flows through a mini funnel and en-
rapid vaporization of the sample and deliver a uni- counters a glass cup. The flow path then inverts
form vapor cloud to the split point. The low mass twice before reaching the split point.
of the wool fiber promotes complete vaporization. Benefits:
Benefits: • Tortuous flow path aids in sample vaporization.
C • Low cost. • Minimizes molecular weight discrimination.
• Reproducible performance. • Can be packed with wool to trap particles.
Drawbacks: Drawbacks:
• Wool can be adsorptive, especially if fibers are • Difficult to clean.
broken.
D • High maintenance requirements. E) Cyclosplitter® (Patent #: 5,119,669)
This patented design incorporates a cylindrical
B) Laminar Cup Splitter glass spiral in the sample pathway, providing a
The sample flows through a small opening and en- large area for sample vaporization.
counters the head of the elongated glass cup. It Benefits:
then travels around the outside of the elongated • Ideal for dirty samples.
E cup before the flow is inverted twice. Larger vol- • Allows many injections of dirty samples before
ume injections are possible because the liquid is cleaning is required.
trapped at the inner base and cannot escape until • Easy to clean.
vaporized. Drawbacks:
Benefits: • Not recommended for large volume injections.
F • Recommended by chromatography expert
Dr. Konrad Grob1. F) Baffle Splitter
• Best splitter liner for high molecular weight The baffle induces turbulent flow that directs the
compounds. sample against the wall of the glass liner.
• Laminar flow profile provides highest Benefits:
resolution. • Reproducible performance.
Drawbacks: Drawbacks:
• Costly. • Prone to molecular weight discrimination.
• Septum particles and residue can enter column.
C) Frit Splitter • Subject to incomplete vaporization.
The sample must pass through the porous ceramic
frit. The high surface area and tortuous flow path
ensure complete vaporization. all liners are
Benefits:
• Traps septum particles and residue.
Drawbacks:
100%
deactivated
• Ceramic frit can be active. See page 17.
• Difficult to clean.
All Restek liners are deactivated to prevent
adsorption of active compounds. Call for
information on custom deactivations.

1
“Injectors Providing Complete Sample Evaporation Above the Column Entrance in Vaporizing GC Injec-
tions,” K. Grob and C. Wagner, HRC & CC, Vol. 16, p. 429.

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7

Operating in the Splitless Injection Mode


When operating in the splitless injection mode (Figures 3 and 4), the solenoid valve is
switched, changing the flow path of the carrier gas. At the beginning of a splitless injection,
the solenoid valve is set to prevent the flow of carrier gas from the injection port body through
the solenoid valve. When the solenoid valve is in this position, only the column flow moves
through the injection port liner. Column flow rate is determined by the pressure of the carrier
gas in the injection port as set by the pressure regulator and the analytical column dimensions.

Figure 3. Figure 3.
Splitless injection flowpaths (injector purge off) in a typical • Solenoid valve closed between injector
flow-controlled/backpressure-regulated system. and split vent: only column flow enters
flow injector; column flow passes into column.
controller injection needle
port valve • Needle valve at septum purge vent allows
only septum purge flow to exit septum
carrier septum purge vent: most of carrier gas diverted
gas purge vent through solenoid valve, out through split
inlet vent.
o-ring or
ferrule split vent
• Sample vapor in injector liner can exit
closed only to column, mixed with column flow
injector 3-way
solenoid of carrier gas.
liner
valve
backpressure • Solenoid valve switched to establish
regulator flowpaths as in split injection: sample
vapor remaining in injection port swept
analytical
column out of split vent.
to detector • Splitless hold time determined by sample
composition.

Figure 4. Figure 4.
Splitless injection flowpaths in a typical headpressure-regulated system. • Solenoid valve closed: entire carrier gas
flow and entire sample directed onto
pressure
throttling regulator analytical column.
needle
valve valve • Carrier gas flow rate into system reduced
injection port
to enable entire flow to pass through
carrier inlet septum analytical column.
purge vent
closed
split vent

solenoid needle
o-ring or valve valve
ferrule
injector
liner
column

to detector

After a carefully determined time (the splitless hold time) the solenoid valve is switched to
re-establish the flow paths as used in the split injection mode. This allows any vaporized
sample remaining in the injection port to be quickly swept out of the injection port liner
through the split vent. A typical splitless hold time is between 60 and 90 seconds. The ideal
splitless hold time is long enough to allow most of the vaporized sample in the injection
port liner to be transferred to the analytical column. Excessively long splitless hold times
can produce tailing peaks and broad peaks. The splitless hold time must be determined
through experimentation, and will vary according to sample composition, column length and
www.restekcorp.com
8

Table II. Typical splitless hold times.

Column Flow Rate Sample Transfer Time*


Column ID Hold Time He H2 He H2
0.18mm 2 min. 0.3cc/min. 0.6cc/min. 2.7 min. 1.4 min.
0.25mm 1 min. 0.7cc/min. 1.4cc/min. 1.2 min. 0.6 min.
0.32mm 0.75 min. 1.2cc/min. 2.4cc/min. 0.7 min. 0.4 min.
0.53mm 0.5 min. 2.6cc/min. 5.2cc/min. 0.3 min. 0.2 min.

*2µL of liquid methylene chloride expanded to 0.8mL vapor at 250°C (10psig headpressure).

ID, carrier gas flow rate, and injection port liner configuration. Table II lists approximate
splitless hold times for various column IDs when operated with helium or hydrogen. The
splitless hold time will decrease as either the column ID or column flow rate increases.

Setting an optimal splitless hold time also is dependent on the choice of sample solvent and
the sample size. Use Table III to estimate the volume of vapor produced when using differ-
ent solvents at different pressures. The volume of vapor cloud formed should be divided by
the column flow rate to determine the approximate time needed to keep the solenoid valve
closed for complete sample transfer. The calculated splitless hold time also should be evalu-
ated to provide the optimum response for the sample analytes. If the solenoid valve is

Table III.
Solvent expansion volumes.
Expansion Volume in µL
at various column headpressures
Solvent Density (g/mL) MW 5psig l0psig 15psig
Heptane 0.68 100 219 174 145
Hexane 0.66 86 245 196 163
Pentane 0.63 72 280 224 186
Toluene 0.87 92 303 242 201
Ethyl acetate 0.90 88 328 261 217
Chloroform 1.49 119 400 319 266
Methylene chloride 1.33 85 500 399 332


Methanol 0.79 32 792 629 525

For customer service, call H2O 1.00 18 1776 1418 1179

800-356-1688, ext. 3 The expansion volumes were determined using a 1.0µL injection volume, a 250° C injection port tem-
perature, and a headpressure of 5, 10, or 15psig (common operating pressures for 30m columns hav-
(814-353-1300, ext. 3) ing IDs of 0.53, 0.32, or 0.25mm, respectively). For 2µL injections, double the expansion volumes.
or call your local Use these formulas to calculate values not listed in Table III:
Restek representative. Expansion volume = nRT / P Online Backflash Calculator:
n= number of moles of solvent and sample.
= [volume (mL) × density (g/mL)] / mol. wt. (g/mole) http://www.restekcorp.com/calculators/backflash.htm
R= gas law constant
= 82.06cc atm/mole °K
T= absolute temperature of injector (°K)
(°K = °C + 273)
P = absolute column headpressure = gauge pressure (atm) + 1 atm
atm = psig × 0.06804 atm / psig

injector liner volume* = πr2L


π = 3.14
r = liner internal radius (cm)
L = liner length (cm)
*Also use this formula to determine capillary column internal volume.

www.restekcorp.com
9

opened too quickly, responses will be low. However, if the solenoid valve remains closed
too long, the solvent peak will tail and peak resolution will suffer. To help determine the Figure 5.
optimal splitless hold time, a series of injections should be made using increasingly longer Optimization of splitless hold time.
splitless hold times. When the response for the analytes of interest plateaus, the sample
transfer process has been optimized (Figure 5). The splitless hold time is optimized
when further increases do not increase analyte
Setting the injection port temperature for splitless injections is critical, just as it is for split response but result in solvent tailing.
injections. The injection port temperature must be high enough to completely vaporize the
sample, yet not so high that it causes sample degradation. This is especially important
because the residence time for a sample in the injection port during splitless injections is
longer, compared to split injections.
Solvent Focusing and Analyte Focusing

area
The long residence time for samples in the injection port also affects peak shape. In splitless
injections, samples are transferred to the head of the column over a longer period of time
than in split injections. As a result, initial peak bandwidths can be very broad unless vapor-
ized samples are refocused at the head of the column. Two techniques can be used to refo-
cus vaporized samples at the head of the column: solvent focusing and analyte focusing.
The difference between the two methods is the initial temperature of the column oven. For
solvent focusing, the initial oven temperature is low enough to allow the solvent to recon- hold time (sec.)
dense at the head of the column. This forms a zone of liquid solvent that traps all of the
vaporized sample analytes in a narrow band at the head of the column. Analyte focusing
requires an initial oven temperature that allows the solvent to move through the column as a
vapor immediately after injection. Analytes that have a significantly higher boiling point
than the solvent are recondensed at the head of the column because of the lower oven
termperature.

A typical sequence of events for performing a splitless injection using solvent focusing is as
follows:

1. Set the initial oven temperature approximately 20°C below the boiling point of the sam-
ple solvent.
2. Close the solenoid valve to divert the entire sample onto the head of the column.
3. Inject the sample and hold the oven temperature at the initial temperature to recondense
the solvent and focus the sample at the head of the column. The initial oven temperature
is typically held for the same amount of time that the solenoid valve is closed.
4. Switch the solenoid valve to open the flow path to the split vent line and rapidly program Split and Splitless Injection in
the oven temperature (10 to 30°C/min.) until the first analyte of interest elutes.
Capillary GC, 4th Ed.
5. Slow the oven program rate to enhance resolution of the remaining analytes of interest. This comprehensive handbook of split
and splitless injection techniques has
been totally revised and updated, con-
taining information on sample evapo-
ration in the injector, matrix effects,
and a new chapter on injector design.
It also includes a CD-ROM contain-
ing visualization of the evaporation
process during split and splitless
injection.

K. Grob, Wiley-VCH, 2001, 460pp.,


ISBN 3-527-29879-7
cat.# 20451 (ea.)

www.restekcorp.com
10

The sequence of events for analyte focusing is the same, except for the initial oven tempera-
Figure 6. ture; instead of starting 20°C below the boiling point of the solvent, the oven temperature is
Initial oven temperature too high for started 60–80°C below the boiling point of the earliest eluting compound.
improper solvent focusing: solvent peak
and early eluting compounds are tailing. Figure 6 shows an example of improper solvent focusing. The sample solvent is hexane,
which has a boiling point of 69°C. The initial oven temperature is 150°C, or 80°C above the
boiling point of hexane. The solvent peak is tailing, and the early-eluting compounds have
broad peak shapes and are poorly resolved from one another. Figure 7 illustrates proper sol-
vent focusing. The initial oven temperature, 40°C, is well below the boiling point of hexane.
The square solvent peak is a good indicator of proper solvent focusing. Also notice the sharp
peak shapes for both early- and late-eluting compounds. When the solvent is not detected or
elicits a low response, such as hexane with electron capture detectors (ECDs), the only indi-
cation of proper solvent focusing is narrow peaks for early-eluting compounds.

For optimal solvent focusing, choose a solvent that has a boiling point at least 20°C below
the boiling point of the earliest eluting target analyte. In some cases, it is not possible to
select the perfect solvent to achieve focusing. For example, methylene chloride (boiling
30m, 0.25mm ID, 0.25µm Rtx®-5 (cat.# 10223) point 40°C) is frequently used for splitless work because of sample preparation techniques.
1.0µL splitless injection of a pesticide mix in Analyses performed with an initial oven temperature of 40°C will not allow the solvent to
hexane (5ng/µL); recondense at the head of the column and will not refocus the sample analytes. Ideally, ana-
Oven temp.: 150°C to 275°C @ 4°C/min.
lysts would start the oven temperature at 20°C when using methylene chloride as the sample
solvent, but because this is not practical, they must rely more on analyte focusing to refocus
sample analytes at the head of the column.
Figure 7. An important part of solvent focusing is the ability of the solvent to “wet” the stationary
Initial oven temperature at least 20°C phase in the column. Non-polar solvents should be used for splitless injections on non-polar
below boiling point of earliest stationary phases (e.g., use hexane or isooctane for injections on Rtx®-1 and Rtx®-5
eluting analyte: early eluting compounds columns). Non-polar solvents are more soluble in non-polar stationary phases and will form
are symmetrical. a more efficient zone of recondensed solvent in the column. Polar solvents are not as soluble
in non-polar stationary phases and will bead up on the stationary phase rather than forming
an even layer of recondensed solvent at the head of the column. Mismatches between the
polarity of the solvent and the polarity of the stationary phase can cause band broadening,
peak splitting, and poor resolution.

Once again, the same basic procedures are followed for analyte focusing, except the initial
oven temperature is 60–80°C below the boiling point of the earliest eluting compound,
instead of 20°C below the boiling point of the solvent, as with solvent focusing.

A unique situation with Agilent 5890 and Double gooseneck inlet liner minimizes
30m, 0.25mm ID, 0.25µm Rtx®-5 (cat.# 10223)
1.0µL splitless injection of a pesticide mix in 6890/6850 split/splitless inlets makes a double the catalytic effects of sample contact
hexane (5ng/µL); Oven temp.: 40°C to 150°C gooseneck liner highly desirable for samples with the metal disk in an Agilent inlet.
@ 25°C/min. then to 275°C @ 4°C/min. that contain compounds prone to catalytic deg-
radation through contact with hot metal sur-
faces. Agilent splitless inlets contain a metal
seal at the base of the inlet (just under the liner
outlet). Because the column is installed only a
few millimeters above the seal surface, the sam-
splitless double
ple contacts the seal while it is being slowly liner gooseneck
drawn into the column. A double gooseneck liner
inlet liner minimizes contact between the sam-
ple and the metal seal. A dirty seal increases the inlet
breakdown of endrin (a pesticide prone to de- seal
composition) from 6% to 12.8% in an Agilent
5890 inlet when a 4mm straight inlet liner is
installed. However, when a double gooseneck
inlet liner is used, the breakdown remains at 2%
regardless of whether the seal is clean or dirty. Endrin Breakdown
(For more information, see page 24 of this
Liner Type Clean Seal Dirty Seal
guide for a description of our Vespel® Ring Inlet
Seal.) Splitless with Wool 6.0% 12.8%
Double Gooseneck 2.0% 2.4%

www.restekcorp.com
11

Inlet Liners for Splitless Injections


The residence time of the sample in a splitless liner is between 0.5 and 2 minutes, so splitless all liners are
inlet liners do not require large surface areas for efficient vaporization (unless you are using
a rapid-injecting autosampler). Splitless liners usually are designed as straight tubes. Alterna-
tive splitless liner designs, such as gooseneck restrictions, help contain the sample cloud in
100%
deactivated
the injector and minimize the breakdown of compounds sensitive to catalytic decomposition See page 17.
on metal inlet parts. Splitless liners should be packed with wool or fused silica beads to help All Restek liners are deactivated to prevent
with vaporization, trap non-volatile residue, and prevent column contamination when analyz- adsorption of active compounds. Call for
ing dirty samples. Some of the more commonly used splitless liners are described below. information on custom deactivations.

A) Straight Tube F) Drilled Uniliner® A


Use for samples containing a narrow molecular This direct injection liner features a hole drilled
weight distribution and for those not prone to into the inlet end that reduces sample discrimina-
thermal decomposition. Packing with wool is rec- tion, compared to typical splitless injections.
ommended. Wool aids in vaporization of high Benefits:
molecular weight compounds and minimizes dis- • Excellent transfer of analytes to column.
crimination. • Decreases injection port discrimination. B
Benefits: • Removes excess solvent vapor.
• Low cost. • Eliminates the need for wool.
Drawbacks: • No sample contact with metal parts below liner,
• Potential decomposition of active compounds less adsorption.
such as endrin and phenols when packed with Drawbacks: C
wool. • Higher amounts of non-volatile materials
• Prone to high molecular weight transferred to column.
discrimination.
• Sample exposed to metal surface below liner. G) 4mm Splitless with Fused Silica Wool
The wool provides a large surface area to allow
B) Gooseneck rapid vaporization of the sample and deliver a uni- D
form vapor cloud to the split point. The low mass
C) Recessed Gooseneck
of the wool fiber promotes complete vaporization.
Benefits:
Benefits:
• Increases splitless efficiency.
• Low cost.
• Decreases breakdown of active compounds
• Reproducible performance.
such as endrin and DDT.
Drawbacks: E
• Chamber contains sample vaporization cloud.
• Wool can be adsorptive, especially if fibers are
• Can be packed with wool.
broken.
Drawbacks:
• High maintenance requirements.
• No known drawbacks.
D) Double Gooseneck F
E) Recessed Double Gooseneck
Best liner for catalytically labile or high molecu-
lar weight compounds. Isolates sample from
metal injection port parts. Use the cyclo-version
for dirty samples. G
Benefits:
• Highest splitless efficiency.
• Breakdown of active compounds decreased.
• Chamber contains vaporization cloud.
Drawbacks:
• Higher cost than straight splitless liners.
• Only recessed double goosenecks can be packed
with wool.

Note: Recessed gooseneck liners offer the same


benefits as single or double gooseneck liners, but
the base of the recessed gooseneck can be packed
with wool and the liner can be used for dual-col-
umn analysis with a two-hole ferrule.

www.restekcorp.com
12

Septum Purge Optimization


The septum purge (Figure 8) serves two func-
Figure 8. tions: to sweep septum bleed volatiles out of
Typical carrier gas flowpath in a the system and to reduce the potential for
Varian split injector. sample backflash contaminating the carrier
gas inlet line. Optimization of the septum
septum purge purge flow rate is important, especially when
out the inlet is operated in the splitless mode.
Most GC manufacturers recommend that the
ferrule
septum purge flow rate be set between 3 and
5cc/min. Flow rates exceeding 5cc/min.
should not be used because highly volatile
carrier gas in sample components could be preferentially
purged from the inlet liner buffer volume after
vaporization. Flow rates lower than 3cc/min.
can allow septum bleed to enter the inlet liner
split vent out and cause ghost peaks to appear on the chro-
split liner
matogram.

split point The septum purge flow rate must be readjust-


ed each time the injection pressure is changed
by more than 5psig. Most GCs have a low-
flow needle valve that makes septum purge
spring
adjustments easy.
column

Figure 9.
Injector temperature affects the recovery of higher molecular weight compounds.

1. naphthalene
2. acenaphthylene
Injector temp: 200°C 3. acenaphthene Injector temp: 300°C
4. fluorene
5. phenanthrene
6. anthracene
7. fluoranthene
8. pyrene
9. benzo(a)anthracene
10. chrysene
11. benzo(b)fluoranthene
12. benzo(k)fluoranthene
13. benzo(a)pyrene
14. indeno(1,2,3-cd)pyrene
15. dibenzo(a,h)anthracene
16. benzo(ghi)perylene

GC_EX00600 GC_EX00601

®
Rtx -5 15m, 0.32mm ID, 1.50µm (cat.# 10266)
Sample: 50µg/mL PAH standard (cat.#31011 ) in hexane
Inj.: 1.0µL splitless (hold 2 min.),
4mm single gooseneck inlet liner w/FSwool (cat.# 22405)
Inj. temp.: 200°C
Carrier gas: helium, constant pressure
Linear velocity: 76cm/sec. @ 40°C
Oven temp.: 40°C(hold 4min.) to 325°C @10°C/min. (hold 5 min.)
Det.: FID @350°C

www.restekcorp.com
13

Figure 10.
The Donike Test illustrates the importance of injector temperature when a sample
contains thermally labile compounds.

1. TMS tetracosanoate (thermolabile) 1 2


2. n-triacontane (stable) 2 3
3. TMS hexacosanoate (thermolabile)
15m x 0.32mm ID fused silica coated with
0.25µm bonded methyl silicone
Sample: 1µL each of TMS n-tetracosanoate, 1
TMS n-hexacosanoate, and n-triacontane in n-
nonane at 2ng/µL each component. 3
GC: 3000 Series Varian gas chromatograph
with 1077 split/splitless injector, FID and
autosampler.
Split/splitless injector:
Run 1: SPI held at 280° C
Run 2: SPI held at 200°C
Carrier gas: helium at 47cm/sec.
Oven: 130° to 280°C 20°C/min. (hold 2 min.)
FID: 300°C, 32 x 10-12

Chromatograms courtesy of Varian 280°C: Injector too hot, 200°C: Injector tempera-
Instrument Co. thermal degradation evident ture appropriate, break-
down minimized

Problems Associated with Split and Splitless Injections


When performed properly, split and splitless injections are easy to automate, produce nar-
row peaks, and yield consistent run-to-run peak areas. However, split and splitless injections
have inherent limitations associated with vaporizing the sample in a hot injection port.

Thermal Decomposition: The injection port temperature is a critical factor in optimizing


hot vaporization injection techniques. If the injection port temperature is too low, high
molecular weight analytes will not vaporize completely and will not be transferred to the
head of the column efficiently (as shown by peaks 14, 15 and 16 in Figure 9). If the injec-
tion port temperature is too high, thermally labile compounds can break down inside the
injection port before reaching the column. Figure 10 shows the effect of temperature on
thermally labile TMS derivatives of fatty acids. When the injection port temperature is set at
280°C, the response for the TMS derivatives is reduced. When the injection port tempera-


ture is lowered to 200°C, the response for the TMS derivatives is comparable to triacontane
at equivalent sample concentrations. Careful optimization of injection port temperatures will For customer service, call
maximize sample vaporization while minimizing sample decomposition. 800-356-1688, ext. 3
Active Compounds: Active compounds can be problematic in split or splitless injections. (814-353-1300, ext. 3)
The high surface area and heat needed to uniformly vaporize the sample can cause these or call your local
compounds to break down or be adsorbed onto the surface of the injection port liner.
Restek representative.
Deactivated inlet liners, and Silcosteel®-treated or gold-plated inlet seals can help minimize
active sites in the injection port. If tailing peaks and poor response for active compounds
cannot be corrected by using properly deactivated inlet liners and treated inlet seals, other
injection techniques such as cold on-column or temperature-programmed injections should
be considered.

Molecular Weight Discrimination: In hot vaporization injections, one injection port temper-
ature is used to vaporize all of the analytes in one sample injection. Compounds spanning a
range of molecular weights and boiling points will exhibit differences in response for equal
concentrations of analyte. High molecular weight, high boiling point analytes will have a
noticeably reduced response when compared to lower molecular weight, lower boiling point
analytes. This effect is more pronounced when analyzing samples that have a broad range of
molecular weights and boiling points. Samples containing analytes that are more closely
grouped by molecular weight and boiling point show less molecular weight discrimination.

www.restekcorp.com
14

Figure 11.
Splitter discrimination typical of split and splitless injections.
Splitter discrimination is evident from relatively enhanced peak heights for the early-eluting com-
pounds and diminished peak heights for the later-eluting higher molecular weight compounds. The
same sample analyzed by cold on-column injection shows no discrimination; the peak heights for low
and high molecular weight compounds are truly representative of this sample.

C6

C6
C44
C44

min. 4 12 20 28 36 44 52 min. 4 12 20 28 36 44 52
Discrimination typical of a split or splitless Cold on-column injection provides accurate
injector. Injector temperature: 340°C information. Injector temperature: 40°C.
30m, 0.32mm ID, 0.25µm Rtx®-1 (cat.# 10124) Det. (FID) temp.: 340°C
Inj. volume: 0.2µL Linear velocity: 50cm/sec., hydrogen
On-column conc.: 15ng. Attenuation: 8x10-11AFS
Oven temp.: 40°C to 340°C @ 5°C/min.

Figure 11 demonstrates the molecular weight discrimination experienced when analyzing a


series of hydrocarbons with a broad range of molecular weights (C6 through C44).
Alternative injection techniques, such as cold on-column injection, can be used to minimize
molecular weight discrimination.

Molecular weight discrimination is usually very repeatable. In split and splitless injections,
if the same injection port temperature, carrier gas pressure, sample size and sample solvent
are used for every injection, sample vaporization should be a reproducible process. Any
molecular weight discrimination experienced should be the same from one injection to the
next. Because of this consistency, many analysts choose to ignore molecular weight discrim-
Figure 12. ination unless it compromises overall sensitivity. To help compensate for differences in
Factors in discrimination: high molecular response due to molecular weight discrimination, multiple internal standards can be used to
weight material clinging to the syringe mimic the range of molecular weights and boiling points for the analytes in the sample.
needle and non-homogeneous vapor-
Molecular weight discrimination can be minimized by choosing an injection port liner that
ization of the sample in the inlet liner.
ensures the sample is completely and uniformly vaporized. Inadequate vaporization causes
the sample to approach the head of the column in both the aerosol and vapor states. Aerosol
droplets, consisting predominantly of high molecular weight compounds, can be driven past
syringe the head of the column by the momentum of the carrier gas and will be preferentially swept
out of the injection port and through the split vent. Injection port liners that are packed with
sample liquid glass wool or that incorporate a flow diverting device within their bore assist in vaporizing
the sample and transferring a homogeneous representation to the head of the column.
septum
evaporating Needle Discrimination: During sample injections, the syringe needle undergoes some
solvent and degree of heating in the injection port. The temperature reached by the needle can influence
needle
volatile solutes the relative response for low and high molecular weight analytes. During the process of
expelling the sample from the syringe, the contents in the needle are not completely trans-
vaporizing residual layer ferred to the injection port. As the needle begins to heat, low molecular weight analytes
chamber of high-boiling begin to vaporize from the needle while higher molecular weight analytes remain inside the
point materials
needle. Therefore, the lower molecular weight analytes will show enhanced response com-
pared to higher weight analytes (Figure 12). Three techniques can be used to minimize nee-
high boiling
materials dle discrimination in split and splitless injections.
(aerosols)
The first technique is to inject the sample as rapidly as possible. Rapid injections minimize
the amount of time the needle spends in the injection port and reduces the amount of heating
column volatile solutes the needle experiences. When making rapid injections in straight injection port liners for
inlet (vapor state)
split or splitless analysis, the sample can be propelled beyond the inlet of the column and
onto the injector base fitting. Always pack injection port liners with deactivated glass wool
or CarboFrit™ packing, or use a flow diverting device like a laminar cup to assist in sample

www.restekcorp.com
15

Figure 13.
Always pack splitless inlet liners with wool when using rapid injection autosamplers.

20 24 28 32 36 20 24 28 32 36
4mm ID splitless liner without wool 4mm ID splitless liner with wool
may exhibit fronting peaks. eliminates fronting peaks by promoting
sample vaporization.

vaporization. Figure 13 shows the improvement in peak shape when an HP autosampler is


used with an injection port liner packed with wool, versus a liner without wool.

The second technique is to use hot needle injection. Hot needle injections are performed by
drawing the sample all the way into the syringe barrel, leaving the needle empty. When the
needle is introduced into the injection port the injection in delayed for a short period of time
(3–5 seconds, for example) to allow the needle to heat completely. Then the syringe plunger
is depressed and the sample is expelled into the injection port liner.

The third technique is to use a solvent flush with each injection. This technique involves
drawing a small amount of solvent into the syringe, followed by a small amount of air, fol-
lowed by the desired amount of sample. All of the solvent, air, and sample are then drawn
into the barrel of the syringe, just as in a hot needle injection. The needle is preheated, as in
the hot needle injection, and the contents of the syringe are expelled into the injection port
liner. The solvent that was first drawn into the syringe acts to flush the syringe barrel and
needle, and completely transfers all of the sample during the injection process.

Backflash: Backflash occurs when the volume of the vaporized sample exceeds the volume
inside the injection port liner. Most of the excess vaporized sample escapes out the top of
the injection port liner. Some of it is swept down the septum purge line. Another portion of
it can back up into the carrier gas supply line, and some of it can be re-introduced into the
injection port. Backflash can cause poor peak area reproducibility, tailing peaks, split peaks,
and poor resolution.

Table III (page 8) shows the estimated expansion volumes for 1µL injections of a variety of
solvents. When using an injection port temperature of 250°C and a carrier gas pressure of
10psig, most solvents will vaporize and expand to a volume that exceeds the capacity of a Table IV.
2mm ID injection port liner (approximately 240µL, see Table IV). In order to minimize Liner Volumes.
backflash, injection port parameters must be carefully optimized. Injection port temperature, Theoretical* Effective
carrier gas pressure, sample size, and rate of injection all should be adjusted to ensure the 1.0mm ID = 59µL 30µL
vaporized sample remains inside the liner prior to being transferred to the head of the col- 2.0mm ID = 236µL 118µL
umn.
3.0mm ID = 530µL 265µL
Sample Size and Injection Port Temperature: As the equation in Table III shows, the vol- 4.0mm ID = 942µL 471µL
ume of vaporized sample produced is directly related to the size of the liquid sample (n) and
the temperature of the injection port (T). A decrease in either of these values will translate *Liner volume actually available for vaporization
with carrier gas present is ≤ 1/2 theoretical, due to
into a smaller vaporized sample volume. If the injection port temperature cannot be the presence of carrier gas in the liner.
decreased because of vaporization problems and the sample size cannot be decreased
because of sensitivity issues, backflash must be minimized by optimizing the rate of injec- From Split and Splitless Injection in Capillary GC,
3rd Ed., K. Grob, Wiley-VCH, 2001.
tion or by adjusting the carrier gas pressure.

www.restekcorp.com
16

Figure 14.
The injection rate must be slower for large volume splitless injections.

5µL/sec. 1µL/sec. 0.2µL/sec.


injection rate injection rate injection rate

1
2 3 4 5

Solvent: Isooctane
1. n-C12
2. n-C14 5µL injection
3. n-C16
4. n-C18 Chromatograms courtesy of Varian Instrument Co.
5. n-C20

Optimizing the Rate of Injection: Figure 14 shows the effect of varying rates of injection for
a 5µL sample. When a rapid injection (5µL/sec.) is made, the solvent peak tails and the
responses for equal concentrations of each analyte are not reproducible. A 1µL/sec. injection
rate improves the solvent peak shape, but the response for each analyte still is not proportion-
al to the concentration of each analyte. Only when the injection rate is slowed to 0.2µL/sec.
does the response for each analyte become consistent with the amount injected.

Some autosamplers are capable of slowing the injection rate to minimize backflash, but
most autosamplers use a rapid injection sequence. If large-volume injections must be made
rapidly, adjustments to the carrier gas pressure must be used to control sample expansion.

Pressure Programming: Pressure (P) is in the denominator of the equation in Table III
(page 8). Any increase in carrier gas pressure will help to reduce sample expansion volume.
Most of the latest models of GCs incorporate electronic pressure control (EPC) of the carrier
gas pressure. Pressure can be time-programmed so that the carrier gas pressure initially is
very high, then is reduced after the injection to optimize carrier gas flow rate for best resolu-
tion. Setting the initial carrier gas pressure to a high value will reduce the amount of sample
expansion that occurs at the point of injection and will speed up the transfer of the vaporized
sample from the liner to the head of the column.

Direct Injection as an Alternative to Splitless Injection


Direct injections are an alternative approach
For customer service, call for injecting samples with low concentrations
Figure 15. of analytes. Direct injections vaporize the
800-356-1688, ext. 3 A Uniliner® liner forms a leak-tight seal entire sample in a heated injection port, just
(814-353-1300, ext. 3) with the column, preventing the sample like split and splitless injections. However, in
from contacting metal parts at the base direct injections, there is only one flow path
or call your local of a splitless injection port. through the injection port. All of the carrier
Restek representative. gas is directed into the column and, hence, the
Uniliner® entire vaporized sample is directed into the
with a column as well. This can be accomplished by
Press-Tight®
splitless using a specially designed injection port liner.
seal
liner Unliner® injection port liners have an internal
taper in one end that allows a direct connec-
inlet seal tion between the liner and the capillary col-
umn. With this connection, the flow path from
the injection port body through the split vent
is blocked and all of the carrier gas flow is
directed into the capillary column. Figure 15
illustrates how a Uniliner® injection port liner
with a Press-Tight® seal forms a leak-free
connection between the liner and the column.

www.restekcorp.com
17

Because all of the carrier gas flow and the entire vaporized sample is directed into the capil-
lary column, direct injections give comparable performance to splitless injections. Faster
carrier gas flow rates usually are used to speed up the sample transfer process, and improve
peak shapes and resolution. Direct injections can be used as another option to minimize
molecular weight discrimination and loss of active compounds.

A Uniliner® inlet liner can be used as a direct replacement for a splitless liner. It can be installed
in the same manner as a splitless liner, except that the system must be operated continuously
with the solenoid valve closed. Uniliner® inlet liners are designed to accommodate 0.32 or
0.53mm ID columns. Request Restek’s Guide to Direct On-Column Vaporization Injection (lit.
cat.# 59882) for more information on how to perform and optimize direct injections.

Standard Gooseneck Uniliner® Inlet Liner

The buffer volume chamber contains the sample vaporization cloud and prevents analyte
contact with metal injector parts. Peak tailing is reduced and larger injections can be made.
Cyclo-Uniliner® Inlet Liner

The glass cyclo spiral provides an excellent vaporization surface for high and low
molecular weight samples. Particles are trapped on the first turn of the spiral, reducing
subsequent residue/sample interaction. In comparison to liners packed with wool, Cyclo-
Uniliner® liners accept up to five times as many injections of dirty samples before cali-
bration curves degrade. Because they are deactivated, they are ideal for active samples.
Open-top Uniliner® Inlet Liner

Open-top Uniliner® liners are ideal for extremely dirty samples because they can be
packed with fused silica wool to trap dirt and sample residue. Contaminated wool is
easily replaced and the liner can be cleaned with a nylon brush or pipe cleaner.
Drilled Uniliner® Inlet Liner

A specially modified injection port liner, developed by Restek chemists, reduces sample
contact with active metal parts in split/splitless injection ports. The Drilled Uniliner® liner
gives the benefits of both direct injection and splitless injection. The column is connected
to the liner by a press-fit connection, thus preventing the sample from contacting the metal


at the bottom of the injection port. The hole on the side of the liner allows the purge flow
to escape from the liner when the injection mode is switched from splitless to split.
For customer service, call
Deactivation 800-356-1688, ext. 3
Siltek Deactivation
™ (814-353-1300, ext. 3)
• Revolutionary deactivation lowers endrin breakdown to less than 1%. or call your local
• Inertness retained over a wide range of sample pH.
• Minimal bleed. Restek representative.
• Recommended for difficult matrix and reactive compound analysis.
• Ideal for chlorinated pesticide analysis.
• Recommended for use with Rtx®-CLPesticides, Stx-CLPesticides, Stx-1HT, and Rtx®-
TNT columns.
Base-Deactivation
• Provides excellent inertness for basic compounds.
• Recommended for use with Rtx®-5 Amine, Rtx®-35 Amine, and Stabilwax®-DB columns.
Intermediate Polarity (IP) Deactivation
Our standard deactivation for liners. Phenylmethyl-deactivated surface provides opti-
mum compatibility for both polar and non-polar compounds.
In most cases, the standard IP deactivation should be chosen. The IP surface contains methyl
groups, as well as phenyl groups, making this surface compatible with most common
solvents.
www.restekcorp.com
18

Hints for Analyzing Dirty Samples


Guard Columns When injecting dirty samples, non-volatile contaminants such as high molecular weight
Guard columns protect analytical
compounds, septum particles, derivatization reagents, salts, and pyrolyzed samples adhere to
columns in several ways:
the interior wall of the injection port liner after the sample solvent and sample analytes have
Guard columns trap non-volatile resi- been vaporized. As this layer of residue thickens, it can cause loss of response for active
dues, preventing them from collecting compounds. Figure 16 illustrates this effect when highly active phenols are analyzed on a
at the analytical column inlet. These clean and a dirty inlet liner. In this example, responses are reduced because of adsorptive
residues may be very high molecular effects in the liner.
weight organic compounds, inorganic
salts, or particles. If these contaminants Figure 16.
enter the analytical column, they can Phenols are adsorbed after several injections of a dirty sample.
cause adsorption of active compounds, 1
1
loss of resolution, and poor peak sym- 1. phenol Initially, phenols respond well
metry. When this contamination begins 2. 2-chlorophenol on a clean, deactivated inlet
3. 2-nitrophenol liner. However, after several
to affect sample analysis, a small sec- 4. 2,4-dimethylphenol injections of Southern
4
tion of the analytical column must be 5. 2,4-dichlorophenol
2
Louisiana crude oil, responses
2 6. 4-chloro-3-methylphenol are greatly diminished due to
removed to restore proper performance. 7. 2,4,6-trichlorophenol the sample’s interaction with
Each time a column section is removed, 8. 2,4-dinitrophenol non-volatile residue in the
9. 4-nitrophenol 4
retention times change, and some reso- 6 inlet liner.
3
10. 2-methyl-4,6-dinitrophenol
lution is lost. By using a guard column 5 11. pentachlorophenol
9
and removing contaminated loops from 3
5
10
it instead of from the analytical column, 7
8
6
11
analytical column length and inertness 7
remain intact. 9
10 11
8
Guard columns also allow more injec-
tions to be made before contamination
min. 4 8 12 16 min. 4 8 12 16
interferes with analytical results.
15m, 0.32mm ID, 1.0µm Rtx®-5 (cat.# 10251)
Because there is no stationary phase 0.2µL split injection of phenols (604 Phenol Mix, cat.# 31029)
coated on a guard column, the amount Oven temp.: 80°C to 290°C @ 8°C/min.
lnj.& det: temp.: 310°C
of time the sample spends in the guard Carrier gas: hydrogen
column is minimal. This reduces the Linear velocity: 45cm/sec.
interaction between sample components FID sens.: 16x10-11
Split ratio: 9:1
and contamination from non-volatile
residue in the guard column.
Non-volatile contamination can be trapped in the injection port liner by using a small plug
For more information on selecting a of deactivated fused silica or glass wool. Usually a 1cm plug of wool, positioned in the cen-
guard column for your analysis, request ter of the injection port liner, is sufficient to provide a surface for non-volatile contamination
our Fast Facts GC Capillary Column to collect. Some instrument manufacturers provide specific instructions on packing injection
Guard Columns (lit. cat.# 59319). port liners to maximize quantitative accuracy and minimize discrimination. If fused silica
wool or glass wool is used in an injection port liner, it should be replaced as part of the rou-
tine maintenance schedule for the injection port. Regular replacement of the wool in the
injection port liner will extend the lifetime of the injection port liner as well as prevent chro-
Mini Wool Puller/Inserter matographic problems from extensive non-volatile contaminant build up. When replacing
Makes inserting and removing wool the wool during routine maintenance, minimize handling of the wool by using a wool puller
easy. Not recommended for double tool (cat.# 20114).
gooseneck liners.
If fused silica or glass wool is not an effective mode of trapping non-volatile contamination
under your conditions, injection port liners with a “cyclo” or glass frit design can be used to
trap non-volatile contamination. While these types of injection port liners may provide
effective trapping of non-volatile contamination, they are harder to clean than straight injec-
tion port liners packed with wool.

In the past, some instruments were supplied with injection port liners that were packed with
a small amount of packed column packing material. We do not recommend using this type
Description qty. cat.# of injection port liner. Diatomites used in packed column GC packings often are active and
Mini Wool Puller/Inserter 2-pk. 20114 contain impurities that increase adsorptive effects for active compounds. Also, the stationary
phases that are used in these packings can produce significant bleed when used in injection
ports at elevated temperatures.
www.restekcorp.com
19

In addition to using a clean and deactivated injection port liner, we recommend using a five-
meter deactivated guard column when analyzing dirty samples. Routine maintenance of the Nylon Tube Brushes and Pipe
liner and the guard column will prevent dirty samples from contaminating the analytical col- Cleaner
umn, and will help ensure reproducible and accurate analytical results. Use to remove small septum fragments
and residue from dirty glass inlet liners.
Hints for Performing Routine Injection Port Maintenance Brushes are 1/8-, 3/16-, and 1/4-inch in diam-
Injection port maintenance should be performed prior to installing any capillary column.
eter; pipe cleaner is one foot long.
Maintenance of the injection port after a column is installed should be performed periodical-
ly, based on the number of injections made and the cleanliness of the samples. Maintenance
includes cleaning, deactivating, or replacing injection port liners, and replacing critical inlet
seals and the septum. Review the instrument manual inlet diagram prior to disassembling
the inlet.
Cleaning and Deactivating Injector Liners
For optimum column performance, the injection port liner must be free of septum particles, Description qty. cat.#
sample residue, and ferrule fragments. Use a deactivated injection port liner when analyzing Nylon Tube Brushes and Pipe
samples with compounds that are active or prone to decomposition or adsorption on untreat- Cleaner set 20108
ed glass surfaces. Table V illustrates the importance of a deactivated injection port liner
when analyzing active compounds. The response factors (RF) for all three of these active
compounds were much lower with non-deactivated inlet liners.
Leak Detective™ II
Leak Detector
• Affordable thermal conductivity leak
Table V.
detector—every analyst can have one.*
Deactivated inlet liners show higher response factors for active components.
• Compact, ergonomic design is easy to
Compound RF Deactivated Liner RF Undeactivated Liner hold and operate with one hand.
RF relative to • Helium, hydrogen, and nitrogen can
2,4-dinitrophenol 0.248 0.185 naphthalene;
pentachlorophenol 0.240 0.188 N=3 be detected at 1x10-4cc/sec. or at an
absolute concentration as low as
benzidine 0.327 0.234
100ppm.**
• Fast results—responds in less than 2
If the injection port liner is deactivated and is not excessively dirty, cleaning with organic seconds to trace leaks of gases with
solvents usually is enough to restore original performance. Most organic solvents will not thermal conductivities different than air.
affect the integrity of the surface deactivation. First, remove septum particles that adhere to • Micro-chip design improves sensitivity
the inside wall of the injection port liner by rinsing with methanol or isopropanol. Next, use and response time over previous models.
pentane, methylene chloride or toluene to remove sample residue. Do not use laboratory • Auto zeroing with the touch of a button.
detergents, acids, or bases to clean injection port liners. Harsh cleaning agents will remove • Battery-operated for increased porta-
or damage the deactivation layer and the liner will require re-deactivation. Nylon brushes bility (one 9-volt).
and pipe cleaners (cat.# 20108) can be used for mild abrasive cleaning of injection port liners.
Replacing Critical Seals
Replace critical seals prior to installing an injection port liner (see the instrument manual for
seal locations). In most capillary injection ports, an o-ring or ferrule made of rubber or
graphite is used to seal the injection port liner into the injection port body. It is critical that
the seal fits tightly around the liner, to prevent the carrier gas from leaking around the out-
side of the liner. Check for leaks with a thermal conductivity-type leak detector (e.g., Leak
Detective™ II, cat.# 20413).
Changing Septa
Always use a high-quality, low-bleed septum. We recommend replacing the septum fre-
quently, to prevent leaks and fragmentation. Multiple injections and continuous exposure to
hot injection port surfaces will decompose the septum and cause particles to fall into the Description qty. cat.#
injection port liner. Septum particles are a potential source of ghost peaks, loss of inertness, Leak Detective™ II Leak Detector
and carrier gas flow occlusion. It is best to install a new septum at the end of an analytical (9 volt, Battery-Operated) ea. 20413
sequence so that it can condition in the injector and reduce the incidence of ghost peaks. To
avoid contamination, always use forceps when handling septa. Restek’s high quality, low- *Never use liquid leak detectors on a capillary sys-
bleed Thermolite® septa are available for most common models of capillary GCs. For more tem because liquids can be drawn into the column.
information, request a copy of Restek’s Guide to Minimizing Septa Problems (lit. cat.# **Caution: NOT designed for determining leaks of
combustible gases. A combustible gas detector
59886).
should be used for determining combustible gas
leaks in possibly hazardous conditions.
For additional hints for analyzing dirty samples, request a copy of Restek’s A Guide When
Injecting Dirty Samples (lit. cat.# 59881). www.restekcorp.com
20

featuring

Siltek™ Deactivation—The Next Generation
20 Siltek
deactivation • Maximizes the inertness of the sample pathway.
• Minimizes breakdown.
• Low bleed.
• Thermally stable.
• “Clean and green”—manufactured without the use of harmful organic solvents.

Restek offers the next generation of deactivation. The Siltek™ deactivation process (patent
pending) produces a highly-inert glass surface, which features high temperature stability,
extreme durability, and low bleed. Try Siltek™ liners, guard columns, wool, and connectors
for better recovery of sample analytes.

For Siltek™ inlet liners, add the corresponding suffix number to your liner catalog
number.
Siltek™ with Siltek™ with
qty. Siltek™ Siltek™ wool CarboFrit™
each -214.1 addl. cost -213.1 addl. cost -216.1 addl. cost
5-pk. -214.5 addl. cost -213.5 addl. cost -216.5 addl. cost
25-pk. -214.25 addl. cost -213.25 addl. cost -216.25 addl. cost

Base-Deactivated Inlet Liners for Agilent GCs


Deactivation—Which If you do not see the deactivated liner you need, you can order it on a custom basis by
Should You Choose? adding the appropriate suffix number to the liner catalog number. For base deactivation:
Siltek™ Deactivation each (-210.1), 5-pack (-210.5), 25-pack (-210.25). For base-deactivated liners packed with
• Revolutionary deactivation lowers base-deactivated wool: each (-211.1), 5-pack (-211.5), 25-pack (-211.25).
endrin breakdown to less than 1%. ea. 5-pk. 25-pk.
• Inertness retained over a wide range 4mm Split Straight w/ Wool
of sample pH. 20781-211.1 20782-211.5 20783-211.25
• Minimal bleed. Cyclosplitter®
• Recommended for difficult matrix 20706-210.1 20707-210.5 —
and reactive compound analysis. 4mm Splitless Straight
• Ideal for chlorinated pesticide analysis. 20772-210.1 20773-210.5 20774-210.25
• Recommended for use with Rtx®- 2mm Gooseneck
CLPesticides, Stx-CLPesticides, 20795-210.1 20796-210.5 20797-210.25
Stx-1HT, and Rtx®-TNT columns. 4mm Gooseneck
20798-210.1 20799-210.5 20800-210.25
Base-Deactivation
• Provides excellent inertness for basic
compounds.
• Recommended for use with Rtx®-5 Prepacked Liners
Amine, Rtx®-35 Amine, and Let Restek do the work! Just add the appropriate suffix to the liner catalog number.
Stabilwax®-DB columns.
Prepacked Inlet Liners Suffix Numbers
qty. FS Wool FS Beads Glass Wool CarboFrit™†
ea. -200.1 -201.1 -202.1 -209.1
5-pk. -200.5 -201.5 -202.5 -209.5
25-pk. -200.25 -201.25 -202.25 -209.25
†CarboFrit™ inserts require a neck greater than 2mm.

For customer service, call


800-356-1688, ext. 3
(814-353-1300, ext. 3)
or call your local

www.restekcorp.com Restek representative.
21
all liners are

100%
deactivated
Liners for Agilent/Finnigan GCs
Splitless Liners
for Agilent/Finnigan GCs Benefits/Uses:
ID**/OD &
Length (mm)
Similar to
Agilent part # ea.
cat.#
5-pk. 25-pk.
2.0 ID 18740-80220
trace samples <2µL 20712 20713 20714
6.5 OD x 78.5 5181-8818
2mm Splitless
4.0 ID
trace samples >2µL 19251-60540 20772 20773 20774
6.5 OD x 78.5
D

4mm Splitless
featuring
™ 4.0 ID
Siltek trace samples >2µL
6.5 OD x 78.5
19251-60540 20772-214.1 20773-214.5 20774-214.25
N

Siltek 4mm Splitless


™ deactivation

4.0 ID
trace samples >2µL 19251-60540 22400 22401 22402
E

6.5 OD x 78.5
4mm Splitless w/ FS Wool
2.0 ID 18740-80220
trace samples <2µL 20914 20915 —
6.5 OD x 78.5 5181-8818
2mm Splitless (quartz)
S

4.0 ID 18740-80220
trace samples >2µL 20912 20913 —
6.5 OD x 78.5 5181-8818
4mm Splitless (quartz)
I

4.0 ID 18740-80220
trace samples >2µL 22403 22404 —
H

6.5 OD x 78.5 5181-8818


4mm Splitless (quartz) w/ FS Wool
2.0 ID
T

trace samples <2µL 5181-3316*** 20795 20796 20797


6.5 OD x 78.5
Gooseneck Splitless (2mm)
featuring
2.0 ID
Siltek ™ trace samples <2µL 5181-3316*** 20795-214.1 20796-214.5 20797-214.25
deactivation
6.5 OD x 78.5
Siltek™ Gooseneck Splitless (2mm)
S

4.0 ID
trace samples >2µL 5181-3316 20798 20799 20800
6.5 OD x 78.5
L

Gooseneck Splitless (4mm)†


featuring

4.0 ID
Siltek trace samples >2µL 5181-3316 20798-214.1 20799-214.5 20800-214.25
L

deactivation 6.5 OD x 78.5


Siltek Gooseneck Splitless (4mm)†

A

4.0 ID
trace samples >2µL 5062-3587 22405 22406 22407
6.5 OD x 78.5
Gooseneck Splitless (4mm) w/ FS Wool†
T

featuring
Siltek ™ 4.0 ID
deactivation trace samples >2µL 5062-3587 22405-213.1 22406-213.5 22407-213.25
6.5 OD x 78.5
Siltek™ Gooseneck Splitless (4mm) w/ Siltek™ Glass Wool†
S

4.0 ID
trace, active samples >2µL 5181-3315 20784 20785 20786
6.5 OD x 78.5
N

Double Gooseneck Splitless (4mm)


featuring
™ trace, active samples >2µL 4.0 ID
Siltek 6.5 OD x 78.5
5181-3315 20784-214.1 20785-214.5 20786-214.25
I

Siltek Double Gooseneck Splitless (4mm)


™ deactivation

trace, active, dirty samples 2.0 ID


— 20907 20908 —
<2µL 6.5 OD x 78.5
Cyclo Double Gooseneck (2mm)
N

trace, active, dirty 4.0 ID


— 20895 20896 20997
samples >2µL 6.5 OD x 78.5
Cyclo Double Gooseneck (4mm)
M

featuring
™ trace, active, dirty 4.0 ID
Siltek
deactivation samples >2µL 6.5 OD x 78.5
— 20895-214.1 20896-214.5 20997-214.25
U

Siltek Cyclo Double Gooseneck (4mm)


base easily packs with wool 2.0 ID


— 20980 20981 20982
for dirty samples <2µL 6.5 OD x 78.5
L

Recessed Gooseneck (2mm)*


base easily packs with wool 4.0 ID
O

— 20983 20984 20985


for dirty samples >2µL 6.5 OD x 78.5
Recessed Gooseneck (4mm)*
featuring
base easily packs with wool 4.0 ID
C


Siltek
deactivation for dirty samples >2µL 6.5 OD x 78.5
— 20983-214.1 20984-214.5 20985-214.25
Siltek™ Recessed Gooseneck (4mm)*
base easily packs with wool 4.0 ID
— 22408 22409 22410
for dirty samples > 2µL 6.5 OD x 78.5
Recessed Gooseneck (4mm)* w/ FS Wool
base easily packs with wool
4.0 ID
for dirty, active samples — 20986 20987 20988
6.5 OD x 78.5
Recessed Double Gooseneck (4mm)* > 2µL
*Use with two-hole ferrule for dual-column analysis. ***Restek design changes improve performance over
**Nominal ID at syringe needle expulsion point. the original Agilent liner.
www.restekcorp.com
†Use this liner for increased sensitivity.
22
all liners are

100% Split Liners


deactivated for Agilent/Finnigan
Liners for Agilent/Finnigan GCs
GCs Benefits/Uses:
ID**/OD &
Length (mm)
Similar to
Agilent part# ea.
cat.#
5-pk. 25-pk.
for purge & trap inlet
1.0 ID
splitting — 20972 20973 —
6.3 OD x 78.5
1mm Split† or sample <1µL
universal, use with
4.0 ID
Agilent 7673 19251-60540 20781 20782 20783
6.3 OD x 78.5
4mm Split with Wool* autosampler
D

featuring universal, use with


™ 4.0 ID
Siltek Agilent 7673
6.3 OD x 78.5
19251-60540 20781-213.1 20782-213.5 20783-213.25
N

deactivation autosampler
Siltek™ 4mm Split w/ Siltek™ Glass Wool
4.0 ID
high MW compounds 18740-80190 20801 20802 —
E

6.3 OD x 78.5
Laminar Cup Splitter
4.0 ID
high MW compounds — 20990 20991 —
6.3 OD x 78.5
mini-Lam™ Split
S

high & low MW 4.0 ID


18740-80190 20709 20710 —
compounds 6.3 OD x 78.5
Cup Splitter
I

featuring

high & low MW 4.0 ID
Siltek 18740-80190 20709-214.1 20710-214.5 —
H

deactivation compounds 6.3 OD x 78.5


Siltek™ Cup Splitter
dirty samples, many
4.0 ID
T

injections before — 20706 20707 20708


6.3 OD x 78.5
Cyclosplitter® cleaning required

dirty samples, trace 4.0 ID


— 21022 21023 20979
samples 6.3 OD x 78.5
4mm Split Precision Liner
S

featuring

Siltek
deactivation
dirty samples, trace 4.0 ID
— 21022-213.1 21023-213.5 20979-213.25
L

samples 6.3 OD x 78.5


Siltek 4mm Split Precision Liner w/ Siltek Glass Wool
™ ™
L

Split/Splitless Liners for ID**/OD & Similar to cat.# cat.#


Agilent 6890 GCs Benefits/Uses Length (mm) Agilent part # ea. 5-pk.
A

universal, use with Agilent 6890 4.0 ID


5183-4647 21032 21033
GCs 6.3 OD x 78.5
Low Pressure Drop Liner w/ Wool
T

DI Liners for Agilent/Finnigan GCs ID**/OD & cat.# cat.#


(For 0.32/0.53mm ID Columns) Benefits/Uses: Length (mm) ea. 5-pk.
S

featuring trace, active samples, 1.0 ID


™ 21052-214.1 21053-214.5
Siltek 1mm Uniliner ***
™ ®
Siltek
deactivation
samples <1µL 6.3 OD x 78.5
N

trace, active samples, high 4.0 ID


20335 20336
recovery & linearity 6.3 OD x 78.5
I

Uniliner®***
featuring
trace, active samples, high 4.0 ID
Siltek ™ 20335-214.1 20336-214.5
deactivation
recovery & linearity 6.3 OD x 78.5
Siltek™ Uniliner®***
N

trace, dirty, high MW active


4.0 ID
samples, high recovery & 20337 20338
6.3 OD x 78.5
Cyclo-Uniliner ***
®
linearity
M

featuring trace, dirty, high MW active


4.0 ID
™ samples, high recovery & 20337-214.1 20338-214.5
Siltek
deactivation linearity
6.3 OD x 78.5
Siltek Cyclo-Uniliner ***
™ ®
U

trace, dirty, active samples, high 4.0 ID


20843 20844
recovery & linearity 6.3 OD x 78.5
L

Open-top Uniliner® with Wool***


DI Liners for Agilent 5890 & 6890 GCs ID**/OD & cat.# cat.#
O

(For 0.25/0.32/0.53mm ID Columns) Benefits/Uses: Length (mm) ea. 5-pk.


allows direct injection when using an 4.0 ID
Hole makes 21054 21055
C

direct EPC-equipped GC 6.3 OD x 78.5


Drilled Uniliner ®

injection
featuring
possible allows direct injection when using an 4.0 ID
Siltek ™ 21054-214.1 21055-214.5
with EPC- deactivation EPC-equipped GC 6.3 OD x 78.5
Siltek™ Drilled Uniliner® equipped
Agilent featuring
allows direct injection when using an 1.0 ID
6890 GCs! Siltek ™ 21390-214.1 21391-214.5
deactivation EPC-equipped GC 6.3 OD x 78.5
Siltek™ 1mm Drilled Uniliner®
*Use with two-hole ferrule for dual-column analysis. ***Restek design changes improve performance over
www.restekcorp.com **Nominal ID at syringe needle expulsion point. the original Agilent liner.
†Use this liner for increased sensitivity.
23

O-Rings
Viton® O-Rings
• For Agilent and PE AutoSys GCs.
• Viton® O-rings fit split (6.3mm OD) or splitless (6.5mm OD) liners.
• Graphite O-rings have excellent thermal stability.
Similar to Restek
Description Max. temp. Agilent part # qty. cat.#
Viton® (fluorocarbon) O-rings 350°C 5180-4182 25-pk. 20377

Graphite O-Rings
• For Agilent and Varian 1177 GCs.
• Excellent thermal stability at injection port temperature up to 450°C!

Similar to Restek cat.#


Description Max. temp. Agilent part # 10-pk. 50-pk.
6.35mm ID Graphite O-rings for split liners 450°C 5180-4168 20296 20297
6.5mm ID Graphite O-rings for splitless liners 450°C 5180-4173 20298 20299

High-Temperature O-Rings
• Stable to 400°C.
• Will not crack or melt.
• Softer and easier to use than graphite.

Description Max. temp. qty. cat.#


High-temperature O-rings 400°C 5-pk. 20437

Inlet and FID Maintenance Kits for Agilent GCs


• Kits include the most common consumable supplies.
• All parts meet or exceed instrument manufacturer’s specifications.
• Includes parts list that makes reordering easy.
Inlet kits include: FID kits include:
• 0.4, 0.5, and 0.8mm ID • 1/4-Inch, 0.4, 0.5, and 0.8mm ID graphite ferrules.
graphite ferrules. • FID/NPD capillary adaptor.
• Viton® o-rings. • Capillary nuts.
• Capillary nuts. • Jet reamers/ferrule removers.
• Inlet seals. • 1/4-Inch nut.
• Reducing nut. • Scoring wafer.
• Scoring wafer. • Capillary column caps.
• 11mm Thermolite® septa. • Ignitor for either Agilent 5890 or 6890/6850 GCs.
• 4.0mm single gooseneck liner.
• FID flow measuring adaptor.
• 4.0mm split liner with wool.
• 1/4- to 5/16-inch wrench.
• Capillary column caps.
• Installation gauge.
• 1/4- to 5/16-inch wrench.
• Septum puller. • Wire cleaning brush.
• Installation gauge. • High-performance Silcosteel®-treated FID jet for
• Wire cleaning brush. either Agilent 5890 or 6890/6850 GCs.
• Jet reamers/ferrule removers. • 1/4-Inch nut driver for jet removal.
• Inlet liner removal tool.
Description qty. cat.#
Inlet Maintenance Kit for Agilent 5890/6890/6850 GCs kit 21069
FID Maintenance Kit for Agilent 5890 GCs kit 21070
FID Maintenance Kit for Agilent 6890/6850 GCs kit 21071
www.restekcorp.com
24

Vespel® Ring Inlet Seals for Agilent 5890/6890 and 6850 GCs
• Easy-to-use, patent-pending design makes a better seal, easily.
• Prevents oxygen from damaging your columns.
• Reduces wear on the injection port body.

In Agilent split/splitless injection ports, it can be diffi-


cult to make and maintain a good seal with a conven- Vespel® ring
minimizes leaks
tional metal inlet disk. The metal-to-metal seal dictates
that the analyst apply considerable torque to the reduc-
ing nut, and, based on our testing, this does not ensure
a leak-tight seal. Over the course of oven temperature
Figure 1 cycling, metal seals are prone to leaks, which ultimate-
The Vespel® Ring Inlet Seal achieves ly can degrade the capillary column, and cause other
leak-tight seals even at low torque, reduc- analytical difficulties.
ing the chance of leaks.
0.01 Our Vespel® Ring Inlet Seal greatly improves injection port performance—it seals even
1E-3 after repeated temperature cycles and without retightening the reducing nut! This seal fea-
stainless steel
Leak Rate (Log10 atm cc/sec.)

1E-4 original equipment tures a Vespel® ring embedded into its face. This soft Vespel® ring will not harm the critical
inlet seal seal on the injector body, and is outside the sample flow path. Tests using a high sensitivi-
1E-5

1E-6 ty helium leak detector indicate the Vespel® Ring Inlet Seal seals equally effectively at
1E-7
torques of 5lb. or 60lb. (Figure 1).
Vespel® Ring Inlet Seal
1E-8
Why trust a metal-to-metal seal when you can make leak-tight seals quickly and easily—
1E-9
and more reliably—with the Restek Vespel® Ring Inlet Seal? Use the stainless steel seal for
1E-10
0 10 20 30 40 50 60
analysis of unreactive compounds. To reduce breakdown and adsorption of active com-
Torque (in. lbs.) pounds, use the gold-plated or Silcosteel®-treated seals. The gold surface offers better inert-
ness than standard stainless steel; Silcosteel® treatment provides inertness similar to that of
fused silica capillary columns.

Vespel® Ring Inlet Seals for Agilent 5890/6890/6850 GCs


0.8mm ID Vespel® Ring Inlet Seal (washers included) 2-pk. 10-pk.
Gold-Plated 21562 21563
Silcosteel® 21564 21565
Stainless Steel 21560 21561
1.2mm ID Vespel® Ring Inlet Seal (washers included) 2-pk. 10-pk.
Gold-Plated 21568 21569
Silcosteel® 21570 21571
Stainless Steel 21566 21567

Re-Threading Tool
• Repair worn or damaged threads.
• Multiple uses (injection ports, fittings, etc.).
• Built-in guide to prevent cross-threading.
1) Worn & damaged threads can
allow oxygen into the sys-
tem—compromising analyti-
1 2 3 cal results and destroying
columns.
2) Screw the tool completely
Achieve a better seal! onto the injection port in a
clockwise direction.
3) Unscrew the tool and inspect
the threads, repeat as neces-
sary, and, when done, wipe
threads with methanol to
remove any debris.

Description qty. cat.#


Re-threading Tool for 1/4" compression fitting
www.restekcorp.com for Agilent split/splitless injection ports ea. 23018
25

Replacement Inlet Seals


• Special grade of stainless steel that is softer and deforms more easily, ensuring a com-
pletely leak-free seal.
• Increases column lifetime because oxygen cannot permeate into the carrier gas.
• Reduced noise benefits high-sensitivity detectors (e.g., ECDs, MSDs).
• Silcosteel® seal offers the inertness of glass.
• All seals include washers.

Replacement Inlet Seals for Agilent 5890/6890/6850 Split/Splitless Injection Ports


The inlet seal at the base of the Agilent 5890/6890 GC injection port contacts the sample
and must be changed frequently to prevent adsorption of active compounds. In addition,
septum fragments and sample residue accumulate on the disk surface, requiring disk
replacement.

The inlet seal design increases column lifetime because oxygen cannot permeate into the
carrier gas. Detector noise also is reduced with high-sensitivity detectors (e.g., ECDs or
MSDs). To reduce breakdown and adsorption of active compounds, use the gold-plated or
Silcosteel® seals. The gold surface offers better inertness than standard stainless steel, and
the Silcosteel® treatment offers inertness similar to that of fused silica capillary columns.

Single-Column Installation, 0.25/0.32mm ID Dual-Column 0.53mm ID Dual-Column Installation


Opening Size 0.8mm ID* Installation, Opening Size 1.2mm ID Opening Size (1/16-inch hole)
2-pk. 10-pk. 2-pk. 10-pk. 2-pk. 10-pk.
Stainless Steel Inlet Seal
21315 21316 20390 20391 20392 20393
Gold-Plated Inlet Seal
21317 21318 21305 21306 — —
Silcosteel Inlet Seal
®

21319 21320 21307 21308 — —


*0.8mm ID stainless steel inlet seal is equivalent to Agilent part #18740-20880,
0.8mm ID gold-plated inlet seal is equivalent to Agilent part #18740-20885.

Replacement Inlet Cross-Disk Seal for Agilent GCs


• Ideal for high-flow split applications on Agilent 5890 GCs.
• All seals include washers.
(Similar to Agilent part # 5182-9652.)

0.8mm ID Cross-Disk Inlet Seal for Agilent GCs 2-pk. 10-pk.


Gold-Plated 20477 20476
Silcosteel® 20475 20474
1.2mm ID Cross-Disk Inlet Seal for Agilent GCs 2-pk. 10-pk.
Gold-Plated 21009 21010
Silcosteel® 21011 21012

www.restekcorp.com
26
all liners are

100%
deactivated
Liners for Varian GCs
Splitless Liners for
Varian 1075/1077 GCs Benefits/Uses:
ID**/OD &
Length (mm)
Similar to
Varian part # ea.
cat.#
5-pk. 25-pk.
2.0 ID
trace samples <2µL 01-900109-05 20721 20722 20723
6.3 OD x 74
2mm Splitless
4.0 ID
trace samples >2µL 01-900109-05 20904 20905 20906
D

6.3 OD x 74
4mm Splitless
trace, active samples 4.0 ID
N

— 20847 20848 20849


up to 4µL 6.3 OD x 74
Double Gooseneck
trace, dirty, active samples 4.0 ID
E

— 20897 20898 —
up to 4µL 6.3 OD x 74
Cyclo Double Gooseneck

Split Liners ID**/OD & Similar to cat.#


S

for 1075/1077 Varian GCs Benefits/Uses: Length (mm) Varian part # ea. 5-pk. 25-pk.
purge & trap inlet splitting 1.0 ID
— 20970 20971 —
I

or samples <1µL 6.3 OD x 72


1mm Split
H

universal, use with rapid autosam- 4.0 ID


01-900109-01 20792 20793 20794
plers 6.3 OD x 72
Splitter with Wool*
T

4.0 ID
high MW compounds 01-900109-02 20803 20804 —
6.3 OD x 72
Laminar Cup Splitter
4.0 ID
high & low MW compounds — 20724 20725 —
S

6.3 OD x 72
Cup Splitter
dirty samples, many injections before 4.0 ID
L

— 20727 20728 —
cleaning required 6.3 OD x 72
Cyclosplitter ®
L

dirty samples, non-active 4.0 ID


01-900109-03 20715 20716 20717
compounds 6.3 OD x 72
Frit Splitter
A

4.0 ID
close boiling compounds 01-900109-04 20718 20719 20720
6.3 OD x 72
T

Baffle Splitter
4.0 ID
dirty samples, active samples — 21030 21031 —
S

6.3 OD x 72
Split Precision™ Liner
N

DI Liners for Varian 1075/1077 GCs ID**/OD & Similar to cat.#


(0.32/0.53mm ID) Benefits/Uses: Length (mm) Varian part # ea. 5-pk. 25-pk.
I

trace, active samples, 4.0 ID


— 20345 20346 —
high recovery & linearity 6.3 OD x 72
Uniliner®
trace, dirty, high MW, 4.0 ID
N

— 20347 20348 —
active samples, linearity 6.3 OD x 72
Cyclo-Uniliner®
trace, dirty, active samples, 4.0 ID
M

— 20845 20846 —
high recovery & linearity 6.3 OD x 72
Open-top Uniliner® with Wool*
U

SPI Liners ID**/OD & Similar to cat.#


for Varian GCs Benefits/Uses: Length (mm) Varian part # ea. 5-pk. 25-pk.
L

high linearity 0.53 ID


01-900109-06 20775 20776 20777
for 0.25 & 0.32mm ID columns 4.6 OD x 54
O

0.5mm SPI
featuring
™ high linearity 0.53 ID 20775- 20777-
Siltek 01-900109-06 20776-214.5
C

deactivation for 0.25 & 0.32mm ID columns 4.6 OD x 54 214.1 214.25


Siltek 0.5mm SPI

high linearity 0.80 ID


01-900109-07 20778 20779 20780
for 0.53mm ID columns 4.6 OD x 54
0.8mm SPI
dirty samples >1µL, fits 0.25, 0.32 & 2.4 ID
01-900109-08 20850 20851 20852
0.53mm ID columns 4.6 OD x 54
SPI with Buffer
*Prepacked with fused silica wool. For glass wool instead, add the suffix “-202” to the liner catalog number.
www.restekcorp.com **Nominal ID at syringe needle expulsion point.
27
all liners are

100%
EN D
deactivated
Liners for Varian GCs
Liners for
Varian 1177 GCs Benefits/Uses:
ID**/OD &
Length (mm)
Similar to
Varian part # ea.
cat.#
5-pk. 25-pk.
4.0 ID
universal 39-26119-36 21045 21046 —
6.3 OD x 78.5
4mm Split
2.0 ID
trace samples <2µL 39-26119-38 — 21077 —
6.5 OD x 78.5
2mm Splitless w/wool*
TH IS

4.0 ID
universal 39-26119-37 — 21079 —
6.3 OD x 78.5
4mm Split w/wool*
1078/1079 Liners ID**/OD & Similar to cat.#
for Varian GCs Benefits/Uses: Length (mm) Varian part # ea. 5-pk. 25-pk.
I N S TALLS

dirty samples, non-active 3.4 ID


03-918464-00 21708 21709 —
compounds 5.0 OD x 54
1078/1079 Split
2.0 ID
trace samples <2µL 03-918466-00 21711 21712 —
5.0 OD x 54
1078/1079 Splitless
featuring
™ 2.0 ID 21711-
Siltek
deactivation
trace samples <2µL
5.0 OD x 54
03-918466-00
214.1
21712-214.5 —
Siltek 1078/1079 Splitless

0.5 ID
trace samples <1µL 03-925331-00 20992 20993 —
5.0 OD x 54
Open 0.5mm ID
3.4 ID
active samples 03-918464-00 20859 20901 20909
C O LU M N

5.0 OD x 54
1078/1079 Split–No Frit
featuring
™ 3.4 ID 20859- 20909-
Siltek
deactivation
active samples
5.0 OD x 54
03-918464-00
214.1
20901-214.5
214.25
Siltek™ 1078/1079 Split–No Frit
0.75 ID
trace, low volume samples 03-925330-00 21714 21715 21716
5.0 OD x 54
Open 0.75mm ID
3.4 ID
trace samples, dirty samples — 21024 21025 —
5.0 OD x 54
1078/1079 Split Precision Liner

*Prepacked with fused silica wool. For glass wool instead, add the suffix “-202” to the liner catalog number.
**Nominal ID at syringe needle expulsion point.

Inlet Liner Seals for Varian 1177 Injectors


Meets original equipment specifications.
(Similar to Varian part # 39-26119-40.)

Description qty. cat.#


Inlet Liner Seals for Varian 1177 Injectors 10-pk. 20298

5mm Liner Seals for Varian 1078/1079 GCs


Description qty. cat.#
5mm Liner Seals for Varian 1078/1079 GCs 10-pk. 22683

Inlet Liner Removal Tool


• Easily remove liners from injectors.
• Made from high-temperature silicone.
• Won’t chip or crack the liner.

Description qty. cat.#


Inlet Liner Removal Tool 3-pk. 20181 No more burned fingers!

www.restekcorp.com
28
all liners are

100%
deactivated
Liners for PerkinElmer GCs
Split Liners
for PerkinElmer GCs Benefits/Uses:
ID**/OD &
Length (mm)
Similar to
PE part # ea.
cat.#
5-pk. 25-pk.
universal, for most 3.5 ID
0330-5181 20736 20737 —
common analyses 5.0 OD x 100
Baffle Splitter
D

high & low MW 3.5 ID


— 20739 20740 —
compounds 5.0 OD x 100
Cup Splitter
N

dirty samples, max.


3.5 ID
injections before — 20745 20746 —
5.0 OD x 100
Cyclosplitter ®
cleaning required
E

3.5 ID
high MW compounds — 20805 20806 —
5.0 OD x 100
Laminar Cup Splitter
universal for most 4.0 ID
S

N6101052 20832 20833 20834


common analyses 6.2 OD x 92.1
Auto SYS Splitter with Wool*
I

featuring
universal for most 4.0 ID
Siltek™ common analyses 6.2 OD x 92.1
N6101052 20832-213.1 20833-213.5 20834-213.25
Siltek™ Auto SYS Splitter w/ Siltek™ Glass Wool deactivation
H

high & low MW 4.0 ID


— 20835 20836 —
compounds 6.2 OD x 92.1
T

Auto SYS Cup Splitter


dirty samples, max.
4.0 ID
injections before — 20910 20911 —
6.2 OD x 92.1
Auto SYS Cyclosplitter ®
cleaning required
S

4.0 ID
high MW compounds — 20827 20828 —
6.2 OD x 92.1
Auto SYS Laminar Cup Splitter
L

dirty samples, trace 4.0 ID


— 21026 21027 —
samples 6.2 OD x 92.1
Auto SYS Split Precision™ Liner
L

Splitless Liners ID**/OD & Similar to cat.#


for PerkinElmer GCs Benefits/Uses: Length (mm) PE part # ea. 5-pk. 25-pk.
A

2.0 ID
trace samples 0330-5180 20730 20731 20732
5.0 OD x 100
T

Splitless (2mm ID)


2.0 ID
S

trace samples N6101372 20829 20830 20831


6.2 OD x 92.1
Auto SYS Splitless w/Wool (2mm ID)*
featuring
Siltek ™
N

2.0 ID
deactivation trace samples N6101372 20829-213.1 20830-213.5 20831-213.25
6.2 OD x 92.1
Siltek Auto SYS Splitless w/Siltek Glass Wool (2mm ID)

I

trace, active samples 4.0 ID


— 20853 20854 —
up to 4µL 6.2 OD x 92.1
Auto SYS Double Gooseneck
trace, dirty, active 4.0 ID
— 20899 20900 —
N

samples, up to 4µL 6.2 OD x 92.1


Auto SYS Cyclo Double Gooseneck

DI Liners for PerkinElmer GCs ID**/OD & Similar to cat.#


M

(0.32/0.53mm ID) Benefits/Uses: Length (mm) PE part# ea. 5-pk. 25-pk.


trace, active samples,
3.5 ID
U

high recovery & — 20855 20856 —


5.0 OD x 100
Uniliner® linearity
trace, dirty, active
3.5 ID
L

samples, high — 20857 20858 —


5.0 OD x 100
Cyclo-Uniliner ®
linearity
O

trace, dirty, active


4.0 ID
samples, high recov- — 20837 20838 —
6.2 OD x 92.1
Auto SYS Open-top Uniliner® w/Wool* ery & linearity
C

trace, dirty, high MW


4.0 ID
active samples, — 20839 20840 —
6.2 OD x 92.1
Auto SYS Cyclo-Uniliner® high linearity
allows direct injec-
4.0 ID
tion when using an — 20819 20822 —
6.2 OD x 92.1
Auto SYS Drilled Uniliner® EPC-equipped GC

*Prepacked with fused silica wool. For glass wool instead, add the suffix “-202” to the liner catalog number.
**Nominal ID at syringe needle expulsion point.

www.restekcorp.com
29
all liners are

100%
deactivated
Liners for Shimadzu GCs
Split Liners for
Shimadzu GCs Benefits/Uses:
ID**/OD &
Length (mm)
Similar to
Shimadzu part # ea.
cat.#
5-pk. 25-pk.
1.0 ID
purge & trap & fast GC — 20976 20977 20978
5.0 OD x 95
17A 1mm Split
universal, for most 3.5 ID
221-25822-01 20751 20752 20753
common analyses 5.0 OD x 128
128mm Split
D

dirty samples, many 3.5 ID


— 20754 20755 —
injections before cleaning required 5.0 OD x 128
128mm Cyclosplitter®
N

high & low MW 3.5 ID


— 20757 20758 —
compounds 5.0 OD x 128
E

128mm Cup Splitter


3.5 ID
high MW compounds — 20807 20808 —
5.0 OD x 128
128mm Laminar Cup Splitter
S

universal, for most 3.5 ID


221-32544-01 20860 20861 20862
common analyses 5.0 OD x 99
99mm Split
I

dirty samples, many 3.5 ID


— 20870 20871 —
injections before cleaning required 5.0 OD x 99
H

99mm Cyclosplitter®
3.5 ID
high MW compounds — 20866 20867 —
5.0 OD x 99
T

99mm Cup Splitter


3.5 ID
high MW compounds — 20868 20869 —
5.0 OD x 99
99mm Laminar Cup Splitter
S

trace samples, dirty 3.5 ID


— 21020 21021 —
samples 5.0 OD x 95
17A Split Precision™ Liner
L

Splitless Liners ID**/OD & Similar to cat.#


for Shimadzu GCs Benefits/Uses: Length (mm) Shimadzu part # ea. 5-pk. 25-pk.
L

3.5 ID
trace samples 221-25440-03 20748 20749 20750
5.0 OD x 128
A

128mm Splitless (3mm ID)


3.5 ID
trace samples 221-32544-00 20863 20864 20865
T

5.0 OD x 99
99mm Splitless (3mm ID)
reduces backflash and catalytic decom- 3.5 ID
S

— 20958 20959 20960


position 5.0 OD x 95
17A 95mm Double Gooseneck
N

reduces backflash, also operates in DI 3.5 ID


221-41599-00 20961 20962 20963
mode 5.0 OD x 95
17A 95mm Single Gooseneck
I

Split/Splitless Liners ID**/OD & Similar to cat.#


for Shimadzu GCs Benefits/Uses: Length (mm) Shimadzu part # ea. 5-pk. 25-pk.
3.5 ID
universal, for most common analyses 221-41444-00 20955 20956 20957
N

5.0 OD x 95
17A 95mm Split/Splitless with Wool*
featuring
Siltek ™ 3.5 ID 20955- 20957-
M

universal, for most common analyses 221-41444-00 20956-213.5


deactivation 5.0 OD x 95 213.1 213.25
Siltek 95mm Split/Splitless w/ Siltek Glass Wool
™ ™

DI Liners for ID**/OD & Similar to cat.#


U

Shimadzu GCs (0.32/0.53mm ID) Benefits/Uses: Length (mm) Shimadzu part # ea. 5-pk. 25-pk.
trace, active samples, high recovery & 3.5 ID
L

— 20872 20873 —
linearity 5.0 OD x 128
128mm Uniliner®
O

trace, dirty, high MW active samples, 3.5 ID


— 20874 20875 —
high linearity 5.0 OD x 128
128mm Cyclo-Uniliner®
C

trace, active samples, high recovery & 3.5 ID


— 20876 20877 —
linearity 5.0 OD x 99
99mm Uniliner ®

trace, dirty, high MW active samples, 3.5 ID


— 20893 20894 —
high recovery & linearity 5.0 OD x 99
99mm Cyclo-Uniliner®
trace, dirty, high MW active samples, 3.5 ID
— 21713 21719 —
high recovery & linearity 5.0 OD x 95
95mm Uniliner® with Wool*
*This liner is prepacked with fused silica wool. To order glass wool instead, add the suffix “-202” to the liner catalog number.
**Nominal ID at syringe needle expulsion point.
30
all liners are

100%
deactivated
D Liners for Thermo Finnigan
Split Liners for
5000-6000 Series GCs Benefits/Uses:
ID**/OD &
Length (mm)
Similar to
TF part # ea.
cat.#
5-pk. 25-pk.
4.0 ID
high MW compounds — 20809 20810 —
5.4 OD x 79.5
Laminar Cup Splitter
N

dirty samples, many


4.0 ID
injections before — 20817 20818 —
5.4 OD x 79.5
E

Cyclosplitter ®
cleaning required

high & low MW 4.0 ID


— 20885 20886 —
compounds 5.4 OD x 79.5
Cup Splitter Gooseneck
S

Splitless Liners for ID**/OD & Similar to cat.#


5000-6000 Series GCs Benefits/Uses: Length (mm) TF part # ea. 5-pk. 25-pk.
I

2.0 ID
trace samples — 20811 20812 20813
5.4 OD x 79.5
Splitless (2mm ID)
H

4.0 ID
trace samples — 20814 20815 20816
5.4 OD x 79.5
T

Splitless (4mm ID)


DI Liners for 5000-6000 Series GCs ID**/OD & Similar to cat.#
(0.32/0.53 ID) Benefits/Uses: Length (mm) TF part # ea. 5-pk. 25-pk.
trace, dirty,
4.0 ID
S

active samples, — 20841 20842 —


5.4 OD x 79.5
Open-top Uniliner® w/Wool* high recovery & linearity
L

Split Liners for ID**/OD & Similar to cat.#


8000 & TRACE™ Series GCs Benefits/Uses: Length (mm) TF part # ea. 5-pk. 25-pk.
L

1.0 ID
purge & trap & fast GC 453 20075 20916 20917 —
8.0 OD x 105
1mm Split
A

3.0 ID
universal 453 20031 20936 20937 20938
8.0 OD x 105
T

3mm Split
5.0 ID
universal 453 20030 20939 20940 20941
8.0 OD x 105
S

5mm Split
4.0 ID
N

high MW compounds — 20948 20949 —


8.0 OD x 105
Laminar Cup Splitter
high & low MW 4.0 ID
I

— 20950 20951 —
compounds 8.0 OD x 105
Cup Splitter
trace samples, dirty 5.0 ID
— 21028 21029 —
samples 8.0 OD x 105
N

5mm Split Precision™ Liner

Splitless Liners for ID**/OD & Similar to cat.#


M

8000 & TRACE™ Series GCs Benefits/Uses: Length (mm) TF part # ea. 5-pk. 25-pk.
3.0 ID
trace samples 453 20032 20942 20943 20944
8.0 OD x 105
U

Splitless (3mm ID)


featuring
™ 3.0 ID
Siltek trace samples 453 20032 20942-214.1 20943-214.5 20944-214.25
L

deactivation 8.0 OD x 105


Siltek Splitless (3mm ID)

O

5.0 ID
trace samples 453 20033 20945 20946 20947
8.0 OD x 105
Splitless (5mm ID)
C

trace active samples up 4.0 ID


— 20952 20953 —
to 4µL 8.0 OD x 105
Double Gooseneck

*Prepacked with fused silica wool. For glass wool instead, add the suffix “-202” to the liner catalog number.
**Nominal ID at syringe needle expulsion point.

www.restekcorp.com
31
all liners are

100% deactivated
Liners for Thermo Finnigan
DI Liners for ID**/OD & Similar to cat.#
COLUMN INSTALLS THIS END

8000 & TRACE™ Series GCs Benefits/Uses: Length (mm) TF part # ea. 5-pk. 25-pk.
trace, active samples,
5.0 ID
high recovery, — 21005 21006 —
8.0 OD x 105
Uniliner® w/Wool & linearity

Split Liners for ID**/OD & Similar to cat.#


TRACE™ 2000 GCs Benefits/Uses: Length (mm) TF part # ea. 5-pk. 25-pk.
trace samples, high 1mm ID
— 21114 21115 —
recovery & linearity 2.95 OD x 120
1mm ID Trace 2000 Glass Liner
2mm ID
universal — 21116 21117 —
2.95 OD x 120
2mm ID Trace 2000 Glass Liner
**Nominal ID at syringe needle expulsion point.

Inlet Liner Seal for TRACE™ 2000 GCs


Description qty. cat.#
Inlet Liner Seal 2-pk. 21392

Graphite Sealing Ring and Washer for 8000 Series and TRACE™ GC
Inlet Liners
(Similar to Thermo Finnigan part # 290-03406)

Description qty. cat.#


Graphite Sealing Ring and Washer ea. 21898
Graphite Sealing Rings and Washers 2-pk. 21899

Graphite Ferrules for M4 Fittings


• High-purity, high-density graphite.
• Smoother surface and cleaner edges than conventional graphite ferrules.
• Contain no binders that can off-gas or adsorb analytes.
• Stable to 450°C.
Graphite Ferrules for M4 Fittings for QCQ Thermo Finnigan 8000 & TRACE™ 2000
Ferrule Fits Column Graphite Graphite
ID ID 2-pk. 10-pk.
0.4mm* 0.18–0.25mm 20280 20281
0.5mm* 0.28/0.32mm 20282 20283
0.8mm* 0.45/0.50 & 0.53mm 20284 20285

*0.4mm ID ferrule is similar to Thermo Finnigan part #290-13488, 0.5mm ID ferrule is similar to
Thermo Finnigan part #290-13487, and 0.8mm ID ferrule is similar to Thermo Finnigan part #290-
13486.

www.restekcorp.com
32

handy Thermolite® Septa


Septum Size Chart • Usable to 340°C inlet temperatures.
• Each batch tested on FIDs, ECDs, and
Instrument Septum Size MSDs to ensure lowest bleed.
Agilent (HP) • Excellent puncturability.
5880A, 5890, 6890,6850 11mm
• Preconditioned and ready to use.
5700, 5880 9.5/10mm
On-Column Injection 5mm • Do not adhere to hot metal surfaces.
CE Instruments (TMQ) • Packaged in non-contaminating glass jars.
TRACE GC 17mm
Finnigan (TMQ) Septum Diameter 25-pk. 50-pk. 100-pk.
GC 9001 9.5mm 5mm (3/16") 20351 20352 20353
GCQ 9.5mm 6mm (1/4") 20355 20356 20357
GCQ w/TRACE 17mm 7mm 20381 20382 20383
QCQ™ 9.5mm 8mm 20370 20371 —
TRACE 2000 9.5mm 9mm 20354 20358 20362
Fisons/Carlo Erba 9.5mm (3/8") 20359 20360 20361
(TMQ) 10mm 20378 20379 20380
8000 series 17mm 11mm (7/16") 20363 20364 20365
Gow-Mac 11.5mm 22385 22386 22387
6890 series 11mm 12.5mm (1/2") 20367 20368 20369
All other models 9.5mm 17mm 20384 20385 20386
PerkinElmer Shimadzu Plug 20372 20373 20374
Sigma series 11mm
900,990 11mm
8000 series 11mm InfraRed™ Septa
Auto SYS 11mm
• Usable to 325°C inlet temperatures.
Auto SYS XL 11mm
Pye/Unicam • Preconditioned and ready to use.
All models 7mm • Excellent puncturability.
Shimadzu • Do not adhere to hot metal surfaces.
All models Plug
SRI
• Low bleed.
All models Plug • Packaged in non-contaminating glass jars.
Tracor
Septum Diameter 25-pk. 50-pk. 100-pk.
540 11.5mm
9mm 21417 21418 21419
550,560 9.5mm
9.5mm (3/8") 21421 21422 21423
220,222 12.5mm
10mm 21424 21425 21426
Varian
11mm (7/16") 21427 21428 21429
Injector type:
11.5mm 21430 21431 21432
Packed column 9.5/10mm
12.5mm (1/2") 21433 21434 21435
Split/splitless
1078/1079 10/11mm 17mm 21436 21437 21438
1177 9mm Shimadzu Plug 21439 21440 21441
1075/1077 11mm
IceBlue™ Septa
• Usable to 250°C inlet temperatures.
• General-purpose septa.
• Excellent puncturability.
• Preconditioned and ready to use.
• Do not adhere to hot metal surfaces.
• Packaged in non-contaminating glass jars.
• Ideal for SPME.
Septum Diameter 50-pk. 100-pk.
9mm 22381 22382
9.5mm (3/8") 22388 22389
10mm 22390 22391
11mm (7/16") 22392 22393
11.5mm 22383 22384
12.5mm (1/2") 22394 22395
17mm 22396 22397
Shimadzu plug 22398 22399

www.restekcorp.com
33

Siltek™ Press-Tight® Connectors


• Siltek™ deactivation for inert pathways to maintain sample integrity.
• Ideal for connecting guard columns to analytical columns.
• Angled Press-Tight® connector designed at an angle approximating the curvature of a
capillary column to reduce strain on column-end connections.
• Fits 0.18, 0.25, 0.32, & 0.53mm ID columns.
Siltek™ Press-Tight™ Connectors
Press-Tight® Connector ea. 3-pk. 5-pk. 25-pk. 100-pk. Siltek™—the most
Universal Press-Tight® Connector — — 20480 20449 20481 inert deactivation available!
Universal Angled Press-Tight® Connector — — 20482 20483 20484
Universal “Y” Press-Tight® Connector 20485 20486 — — —
Universal Angled “Y” Press-Tight® Connector 20487 20469 — — —

Universal Angled Press-Tight® Connectors


• Designed at an angle approximating the curvature of a capillary column.
• Reduces strain on column-end connections.
• Ideal for connecting guard columns to analytical columns.
• Seals all common sizes of fused silica tubing (0.18 to 0.53mm ID, outside diameters
from 0.3 to 0.75mm).
• Made from inert fused silica.
Description qty. cat.#
Universal Angled Press-Tight® Connectors 5-pk. 20446
Universal Angled Press-Tight® Connectors 25-pk. 20447
Universal Angled Press-Tight® Connectors 100-pk. 20448

Universal Press-Tight® Connectors


• Connect guard columns to analytical columns.
• Repair broken columns.
• Connect column outlets to transfer lines.
Description qty. cat.#
Universal Press-Tight® Connectors 5-pk. 20400
Universal Press-Tight® Connectors 25-pk. 20401
Universal Press-Tight® Connectors 100-pk. 20402

Deactivated, Universal Press-Tight® Connectors


• High-temperature silanization for excellent inertness. Polyimide Resin
• Ideal for trace analysis of active compounds. • Permanently connects a Press-
• Ideal for analysis of pesticides, semivolatile pollutants, or clinical/forensic samples. Tight® connector to a fused silica
column.
Description qty. cat.# • 350°C maximum operating temper-
Deactivated, Universal Press-Tight® Connectors 5-pk. 20429
ature.
Deactivated, Universal Press-Tight® Connectors 25-pk. 20430
Deactivated, Universal Press-Tight® Connectors 100-pk. 20431

Universal “Y” Press-Tight® Connectors


• Split sample flow onto two columns.
• Split a single column flow into two detectors—
perform confirmational analysis with a single
injection.
• Fit 0.18, 0.25, 0.32, & 0.53mm ID columns.
Description qty. cat.#
Universal “Y” Press-Tight® Connector ea. 20405
Universal “Y” Press-Tight® Connectors 3-pk. 20406 Description qty. cat.#
Polyimide
Resin 5 grams 20445

www.restekcorp.com
34

MXT®-Union Connector Kits—For Fused Silica Columns


Use for fused silica-to-fused silica or • Low-dead-volume, leak-free connection.
fused silica-to-metal connections! • Reusable.
• Silcosteel® treatment ensures maximum inertness.
• Ideal for connecting guard columns and transfer lines.
• Use to oven temperatures of 350°C.
• Available in union and “Y” configurations.

Previously, easy-to-use MXT® connectors could only be used with metal tubing. Now
MXT® connectors can be used with fused silica capillary columns, because of a Valcon
polyimide 1/32-inch one-piece fused silica adaptor. This unique graphite-reinforced compos-
ite allows capillary columns to slide into and be locked in place simply by loosening and
tightening the MXT® union 1/32-inch fitting.
MXT®-Union Connector Kits—For Fused Silica Columns
Each kit contains the MXT® union, two 1/32-inch nuts and two one-piece fused silica adaptors.
Description qty. cat.#
For 0.25mm ID Fused Silica Columns kit 21386
For 0.32mm ID Fused Silica Columns kit 21385
For 0.53mm ID Fused Silica Columns kit 21384

MXT® “Y”-Union Connector Kits—For Fused Silica Columns


Each kit contains the MXT® union, three 1/32" nuts and three one-piece fused silica adaptors.
Description qty. cat.#
For 0.25mm ID Fused Silica Columns kit 21389
For 0.32mm ID Fused Silica Columns kit 21388
For 0.53mm ID Fused Silica Columns kit 21387

1
/32-Inch Replacement Nut
Description qty. cat.#
1
/32" Replacement Nut 5-pk. 20389

Valco® Connectors—One-Piece Fused Silica Adaptor Ferrule


We recommend a one-piece adaptor ferrule for use in fittings where the ferrule will not be
removed. Connections are made and disconnected by loosening the fitting nut and sliding
the tube out. Fused silica adaptor ferrules are available in Valcon polyimide for use up to
350°C. Valcon polyimide is a unique graphite-reinforced composite, specially prepared to
maximize mechanical stability at high temperatures. The determining factor in adaptor fer-
rule size selection is the fused silica tubing outer diameter (OD).

/32-Inch Adaptor Ferrule


1

Valcon Polyimide
Tubing OD Tubing ID Valco® # qty. cat.#
<0.25–0.4mm 0.25mm FS.4-5 5-pk. 20137
0.4–0.5mm 0.32mm FS.5-5 5-pk. 20140
0.5–0.8mm 0.53mm FS.5V-5 5-pk. 20141
1
/32" Replacement Nut 5-pk. 20389

Gerstel GRAPHPACK® 3D/2 Connectors


GRAPHPACK® technology provides a complete system that quickly and reliably makes
leak-free, low-dead-volume connections. The central component is a metal-jacketed
Ideal for MXT® stainless steel to fused graphite ferrule—the ideal seal for GC applications. GRAPHPACK® ferrules eliminate all
silica capillary connections! the disadvantages and shortcomings associated with previous sealing systems.
Description qty. cat.# GRAPHPACK® 3D/2 Ferrules
GRAPHPACK 3D/2 Connector**
®
Ferrule ID Fits Column ID qty. cat.#
(0.25mm to 0.32mm ID) ea. 20272 0.4mm 0.25mm 10-pk. 20271
GRAPHPACK® 3D/2 Connector** 0.5mm 0.32mm 10-pk. 20270
www.restekcorp.com (0.45mm to 0.7mm ID) ea. 20273 0.8mm 0.45/0.53mm 10-pk. 20274
**Use only with GRAPHPACK® 3D/2 ferrules.
35

Intermediate-Polarity Deactivated Guard Columns & Transfer Lines


• Useful for a wide range of applications.
• Compatible with most common solvents.
Fused Silica Guard Columns/Transfer Lines
Nominal ID Nominal OD 1-Meter 5-Meter 5-Meter/6-pk.
0.025mm* 0.363 ± 0.012mm 10097
0.05mm 0.363 ± 0.012mm 10098 10040 10040-600
0.075mm* 0.363 ± 0.012mm 10099
0.10mm 0.363 ± 0.012mm 10100 10041
0.15mm 0.363 ± 0.012mm 10101 10042
0.18mm 0.37 ± 0.04mm 10102 10046
0.25mm 0.37 ± 0.04mm 10043 10043-600
0.28mm 0.37 ± 0.04mm 10003 10003-600
0.32mm 0.45 ± 0.04mm 10044 10044-600
0.45mm 0.69 ± 0.04mm 10005 10005-600
0.53mm 0.69 ± 0.05mm 10045 10045-600

Nominal ID Nominal OD 10-Meter 10-Meter/6-pk. 30-Meter** 60-Meter**†


0.25mm 0.37 ± 0.04mm 10049 10049-600 10012 10013
0.32mm 0.45 ± 0.04mm 10048 10048-600 10022 10023
0.53mm 0.69 ± 0.05mm 10047 10032 10033

MXT® Guard Columns/Transfer Lines


Nominal ID Nominal OD 5-Meter 5-Meter/6-pk. 10-Meter
0.28mm 0.53 ± 0.025mm 70044 70044-600 70046
0.53mm 0.74 ± 0.025mm 70045 70045-600 70047

Siltek™-Deactivated Guard Columns


• Revolutionary deactivation process lowers analyte breakdown to less than 1%.
• Minimizes bleed.
• Ideal for chlorinated pesticide analysis.
• Analyze tough samples quickly and accurately.
• Maximum temperature of 380°C.
Siltek™-Deactivated Guard Columns
Nominal ID Nominal OD 5-Meter 10-Meter
0.25mm 0.37 ± 0.04mm 10026 10036
0.32mm 0.45 ± 0.04mm 10027 10037
0.53mm 0.69 ± 0.05mm 10028 10038

Let Restek Make the Connection for You!


Restek will connect a Siltek™ guard column to any analytical column using a universal
Siltek™ Press-Tight® connector and polyimide sealing resin. To order a preconnected guard
column, add the three-digit suffix from the chart below to any analytical column catalog
number when ordering.

5m Siltek™ Guard Column/Transfer Line Example: Restek Trademarks: Siltek, Press-Tight, MXT,
CarboFrit, Rtx, Uniliner, Silcosteel, Stx, Leak Detective,
A 5m, 0.32mm ID Siltek™ guard column Stabilwax, Cyclosplitter, mini-Lam, Precision, InfraRed,
ID cat.# suffix
IceBlue, Plus 1.
0.25mm -364 connected to a 30m, 0.32mm ID, 1.0µm
0.32mm -365 Rtx®-5 column is cat.# 10254-365. Other Trademarks: Valco (Valco Instruments Co., Inc.),
0.53mm -366 GRAPHPACK (Gerstel GmbH), Carbowax (Union
Carbide Corp.), TRACE (ThermQuest Corp.), Velcro
*Not tested with the Grob test mix because of a high pressure drop. (Velcro Industries BV), Scotty (Scott Specialty Gases,
**30- and 60-meter lengths are banded in 5-meter sections. Inc.), Viton & VESPEL (E.I du Pont de Nemours & Co.,
†Recommendation: Cut 60m guard columns into shorter lengths. Using full length may cause peak dis- Inc.).
tortion.

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Plus 1Restek’s Customer Commitment
Plus 1™ Service means we will surpass your expectations every time you contact us! You’ll
get Plus 1™ service when you ask our experienced Technical Service team to help solve a dif-
ficult analytical problem. Our efficient Customer Service Team will provide Plus 1™ service
even when you place a late-day order. Keep reaching for Restek products and service, and we
will provide you with Plus 1™ quality and attention.

Orders & Customer Service (in the U.S.)

For customer and technical service outside the U.S.…


please contact your local Restek International location or distributor.

Germany: Schaberweg 23, 61348 Bad Homburg • phone: 49 06172 2797 0 • fax: 49 06172 2797 77
France: 1, rue Montespan, 91024 Evry • phone: 01 60 78 32 10 • fax: 01 60 78 70 90
Ireland: 8 Baronscourt Lane, Belfast, BT8 8RR • phone: 44 28 9081 4576 • fax: 44 28 9081 4576
Thames Restek UK Ltd.: Units 8-16 Ministry Wharf, Wycombe Road, Saunderton, Buckinghamshire, HP14 4HW
phone: 01494 563377 • fax: 01494 564990

©Copyright 2002, Restek Corporation


For permission to reproduce any portion of this technical guide, please contact Restek’s publications/graphics department by phone (ext.
2128) or fax (814) 353-9278.
Lit. Cat. #59880A

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